coatings

Article
Adhesion of Soft Materials to Rough Surfaces:
Experimental Studies, Statistical Analysis
and Modelling
Andrey Pepelyshev 1 , Feodor M. Borodich 2, * , Boris A. Galanov 3 , Elena V. Gorb 4 and
Stanislav N. Gorb 4
1 School of Mathematics, Cardiff University, Senghennydd Road, Cardiff CF24 4AG, UK;
[email protected]
2 School of Engineering, Cardiff University, The Parade, Cardiff CF24 0AA, UK
3 Institute for Problems in Materials Science, National Academy of Science of Ukraine, 3 Krzhyzhanivsky Str.,
Kiev 03142, Ukraine; [email protected]
4 Department of Functional Morphology and Biomechanics, Zoological Institute, Kiel University,
Am Botanischen Garten 1–9, 24118 Kiel, Germany; [email protected] (E.V.G.);
[email protected] (S.N.G.)
* Correspondence: [email protected]

Received: 4 September 2018; Accepted: 27 September 2018; Published: 30 September 2018

Abstract: Adhesion between rough surfaces is an active field of research where both experimental
studies and theoretical modelling are used. However, it is rather difficult to conduct precise
experimental evaluations of adhesive properties of the so-called anti-adhesive materials. Hence,
it was suggested earlier by Purtov et al. (2013) to prepare epoxy resin replicas of surfaces having
different topography and conduct depth-sensing indentation of the samples using a micro-force tester
with a spherical smooth probe made of the compliant polydimethylsiloxane polymer in order to
compare values of the force of adhesion to the surfaces. Surprising experimental observations were
obtained in which a surface having very small roughness showed the greater value of the force of
adhesion than the value for a replica of smooth surface. A plausible explanation of the data was
given suggesting that these rough surfaces had full adhesive contact and their true contact area is
greater than the area for a smooth surface, while the surfaces with higher values of roughness do
not have full contact. Here, the experimental results of surface topography measurements and the
statistical analysis of the data are presented. Several modern tests of normality used showed that the
height distribution of the surfaces under investigation is normal (Gaussian) and hence the classic
statistical models of adhesive contact between rough surfaces may formally be used. Employing one
of the Galanov (2011) models of adhesive contact between rough surfaces, the plausible explanation
of the experimental observations has been confirmed and theoretically justified.

Keywords: micro-roughness; normality tests; force tester; polydimethylsiloxane; epoxy resin;

pull-off force

1. Introduction
Molecular adhesion is a universal physical phenomenon that usually has a negligible effect on
surface interactions at the macro-scale, whereas it becomes increasingly significant as the contact
size decreases [1]. Although the main topic of recent studies of adhesive interactions has been
devoted to materials showing enhanced adhesive properties, the studies of the so-called anti-adhesive
materials are also a growing field of interest. The term ‘anti-adhesive’ is attributed to materials and
coatings showing very low values of adhesive forces. However, anti-adhesive properties should
not be attributed solely to materials having low surface-energy because surface roughness may

Coatings 2018, 8, 350; doi:10.3390/coatings8100350 www.mdpi.com/journal/coatings

Coatings 2018, 8, 350 2 of 17

drastically affect adhesion of surfaces made of the same material (see, e.g., [2–5] and literature
therein). For example, the adhesive force may be very low for some biological and bio-inspired
surface topographies, as they show generic anti-adhesive behaviour due to minimization of the true
contact area.
Evidently, reliable measurements of adhesion properties of surfaces are very important for
understanding of the underlying processes. However, these measurements may be of low precision if
hard spherical probes are used to study surfaces with reduced adhesion. In addition, if the values of
the force of adhesion become very low, then one needs to increase correspondingly the sensitivity of a
testing method for adhesion force measurements. Hence, it was suggested in [5] to use a micro-force
tester combined with a soft spherical probe to conduct depth-sensing indentation (DSI) tests, and to
extract the values of adhesive force for nominally flat surfaces made of the same material and having
different roughness parameters. This experimental scheme has the advantage that there is no difference
between the materials of different samples and therefore the surface roughness is the main factor that
influences the relative values of the force of adhesion.
The experimental studies consisted of several parts: (i) preparation of polymer replica surfaces
and probes followed by indentation tests; (ii) extraction of the standard surface roughness parameters;
and (iii) detailed studies of roughness topography. The first two parts were described in detail in [5]
and [6] and here a brief version of this description will be presented for the sake of completeness. The
last part will be described for the first time in the next chapter along with the statistical analysis of the
surface topography.
The deformable half-spherical indenters were made out of polydimethylsiloxane (PDMS) polymer
applying a replica method to precision sapphire spheres of radius Rs = 1.5 ± 0.0025 mm used as
templates. Then, depth-sensing indentation (DSI) tests were performed. The force tester Basalt 01 (Tetra
GmbH, Ilmenau, Germany) used in the tests was described earlier in several papers (see, e.g., [7–10]).
All measurements were carried out at a constant applied force (Fload = 503.11 ± 23.43 µN). A clean smooth
glass surface and polishing papers of nominal asperity sizes 0.3, 1, 3, 9, 12 µm were used as templates for
preparation of the epoxy resin replicas. The roughness of test surfaces was characterised using a white
light interferometer (Zygo NewView 6000; Zygo Corporation, Middlefield, CT, USA) at a magnification
of 50. Using topographical images, the standard roughness parameters were calculated.
Surprisingly, the highest pull-off force values were obtained not on the smooth sample having
Ra = 0.7 nm, but rather on the surface with some micro-roughness (the nominal asperity size 0.3 µm).
The pull-off forces decreased continuously with the further increase of the surface microroughness.
A plausible explanation of the observations was given in [5]. Assuming that there is almost full contact
between the spherical probe and the tested surface for both the nominally flat sample and the surface
having the nominal asperity size of 0.3 µm, one can expect that the full area of the rough surface may
be greater than the area of the flat sample. This in turn causes the adhesive force for the rough sample
to have full contact higher than for a flat one. On the other hand, for surfaces having more pronounced
roughnesses, partial contacts occur and the real contact area decreases, which causes the adhesive
force to decrease [5]. However, these explanations need to be theoretically justified.
In this paper, the results of statistical analysis of surfaces used in the depth-sensing indentation
experiments [5] are presented. It is shown that these intact surfaces follow the Gaussian law of asperity
height distributions and, therefore, one can use some of the standard models of adhesive contact
between rough surfaces. Here, one of the Galanov models of adhesive contact [11] is employed
for studying contact between rough surfaces. Statistical arguments are presented that support the
above-mentioned plausible explanation of the adhesive force observations.

2. Preliminaries
It is well established that topography of solid surfaces involves finite scale roughness regardless
of preparation method of the surfaces [12–14]. The surface texture plays an important role in adhesion
between surfaces and there are rather complicated relations between surface topography and the
Coatings 2018, 8, 350 3 of 17

values of the adherence force. Evidently, to model adhesion between rough surfaces, one needs to
employ corresponding models [3,11,15]. In turn, there is a need for proper statistical analysis of surface
topography. We give below some preliminary information related to various approaches to description
of surface roughness along with a brief review of models of contact between elastic rough surfaces.
Both adhesive and non-adhesive models are discussed. Special attention is given to models developed
in [3] and two models introduced in [11].

2.1. Statistical Description of Rough Surfaces

Various parameters and functions related to the surface asperity shapes and distributions of the
asperities were suggested to be used as statistical surface characteristics [16]; however, Whitehouse [17]
noted that some of these parameters are useful, but most are not.
Let us consider a nominally flat surface. If one considers a plane perpendicular to the surface,
then the cross-section between the surface and the plane is a profile. Let a function z( x ) describe the
rough profile. The origin level of the height measurements can be taken as the mean profile line z̄.
Then, one has Z L
1
[z( x ) − z̄]dx = 0.
2L − L
The most popular statistical height parameters for a function z( x ) defined on an interval [− L, L]
are the maximum height of the profile Rmax , the arithmetical mean deviation of the surface Ra , and the
square root of the mean square deviation σ2 (the rms height Rq ) with respect to the mean profile line
z̄ = 0
Rmax = max z( x ),
x ∈[− L,L]
1/2
∑n |z( xi )|
Z L  Z L
1 1 2
Ra = |z( x )| dx ≈ i=1 , Rq = σ = [z( x )] dx , (1)
2L −L n 2L −L

where n is the number of points of measurements on the interval and z( xi ) is the measured height
at the interval point xi . In practical calculations, the arithmetic mean height Rz is often used; it is
calculated as the average distance between the five highest picks and the five lowest points of the
profile, i.e., " #
1 5 5

5 i∑
Rz = (zi )max − ∑ (zi )min . (2)
=1 i =1

One can introduce the density probability function φ(z) that shows the probability that the height
z( x ) at a surface point x is between z and z + dz. Then, the expressions for Ra and σ2 in Equation (1)
can be written as Z ∞ Z ∞
Ra = |z|φ(z) dz, σ2 = z2 φ(z) dz. (3)
−∞ −∞
Other popular parameters of roughness include the rms slope or the rms curvature, parameters
associated with horizontal distributions, e.g., the number of intersections of the surface with the
average line, and parameters describing spatial extent of asperities, such as the high spot count, and so
on. It is quite clear that the cumulative distribution function of the surface heights Φ(z) is correlated
with contact properties of the rough surfaces
Z ∞
Φ(z) = φ(t) dt. (4)
z

In tribology, this function is known as the bearing area curve or the Abbott–Firestone curve.
Actually, Abbott and Firestone [18] suggested calculating the integrals of the horizontal line at a
specific level, which lies within the roughness profile. Its value at a level z = h is equal to the length
(the area in the 2D problem) of the slice of the profile at the level h.
Coatings 2018, 8, 350 4 of 17

We have to mention that the original rough surfaces of polishing papers were made using particles
of diameters 0.3, 1, 3, 9, 12 µm and these diameters were used to specify the nominal asperity sizes.
Using the above definitions from Equations (1) and (2), the replica surfaces were examined in [5].
The results obtained are presented in Table 1. The first line is attributed for a replica of smooth glass
surface. As it was defined above, Ra is the roughness average (the absolute value of the surface height
averaged over the surface); rms is root mean square (a statistical value of the magnitude of a varying
quantity) and Rz is determined roughness, i.e., the average of N = 10 extremal roughness heights over
a specified length.

Table 1. Roughness values of tested epoxy resin replicas.

Nominal Size of Surface Asperities (µm) Ra (µm) rms (µm) Rz (µm)

0 0.007 ± 0.001 0.009 ± 0.001 0.069 ± 0.035
0.3 0.150 ± 0.005 0.205 ± 0.006 2.223 ± 0.172
1 0.439 ± 0.016 0.559 ± 0.019 5.998 ± 0.732
3 1.329 ± 0.138 1.685 ± 0.172 11.550 ± 0.633
9 3.073 ± 0.275 3.930 ± 0.297 41.857 ± 5.742
12 3.515 ± 0.554 4.432 ± 0.588 29.432 ± 2.669

The values of Table 1 were obtained using the arrays of discrete values obtained by measurements
in specific points of profiles. However, one can also consider the density probability function of
asperity summits φ(zs ) and the cumulative summit height distribution Φ(zs ). These functions are
used in models of discrete contacts between rough surfaces.
The above characteristics are mainly related to vertical distribution of rough profiles. However,
the horizontal distribution of the profiles is also very important. The surface roughness profiles may
be modelled as graphs of a random process. As early as 1953, Linnik and Khusu delivered a seminar
where they suggested to describe surface roughness using graphs of a stationary Gaussian random
process having a correlation function

K ( x ) = K (0 ) · e−α| x | , (5)

where K (0) and α are some parameters of the roughness (see, for details, an abstract of the seminar [19],
as well as [20] and [13]). Practically all known models of contact between rough adhesive surfaces are
based on explicit or implicit assumption of the Gaussian distribution of heights (see a review in [21]).
The Gaussian distribution has an attractive property that, if the random surface is normal, then it can
be completely described by two parameters: (i) the height distribution and (ii) an auto-correlation
function [14]. The latter function characterizes the horizontal distribution of asperities of a rough
surface profile. Indeed, one needs to specify both vertical and horizontal distributions because, as it
was clearly formulated in [15], two profiles may have the same height and peak height (local extrema)
distributions, but they may differ in the horizontal extension. The profile auto-correlation function is
defined as
Z L
1
R(δ) = lim [z( x + δ) − z̄][z( x ) − z̄] dx = h[z( x + δ) − z̄][z( x ) − z̄]i. (6)
L→∞ 2L −L

Evidently, it is possible to put z̄ = 0 in Equation (6). The correlation (auto-correlation) function is

often substituted by its Fourier transform that is called the spectral density function.
Various mathematical tools are developed to work with surfaces having the Gaussian (normal)
distribution of heights (see, e.g., [13,15]). However, to apply these tools, one needs to demonstrate
that the surface roughness follows the Gaussian law. Quite often, these tools are used without proper
justification that they may be used, while it is not evident that the roughness height distribution
is normal. In fact, the accurate statistical analysis of grinding surface roughness showed that the
distribution is not normal either at micro or nanoscales [21]. Therefore, the results of an accurate
Coatings 2018, 8, 350 5 of 17

statistical analysis of surfaces are presented below. As it has been mentioned, the test surfaces were the
same as described in [5]; namely, these were the epoxy resin replicas of polishing papers produced by
Serva Electrophoresis GmbH (Heidelberg, Germany) with nominal asperity sizes 0.3, 1, 3, 9, and 12 µm
along with a replica of a clean smooth glass surface. The glass surface having Ra asperity roughness of
7 nm was considered as a nominally smooth one.

2.1.1. Non-Adhesive Contact between Rough Elastic Solids

Apparently, the first statistical model of contact between rough surfaces was presented in 1940
by Zhuravlev [22]. He assumed that all asperities are elastic spheres of the same radius R located at
various heights, i.e., it was a statistical multi-level model of roughness. He argued that profiles at a
specific height may be characterized by a distribution function ψ(ξ), i.e., the number of spheres in
contact increases as one considers the deeper levels ξ. Applying the Hertz contact theory, he derived
general expressions for the true contact area A between the surfaces and the contact force P:

πR Rmax /2 Rmax /2
Z Z
A= [δ − (ξ1 + ξ2 )]ψ(ξ1 )ψ(ξ2 )dξ1 dξ2 (7)
2N 0 0
√ Z Rmax /2 Z Rmax /2
2R
P= [δ − (ξ1 + ξ 2 )]3/2 ψ(ξ1 )ψ(ξ2 )dξ1 dξ2 (8)
3πkN 0 0

Here, k = (1 − ν2 )/πE is the effective contact modulus of surfaces having the elastic modulus E and
the Poisson ratio ν, δ is the relative approach due to compression of the surfaces, and N is the total
number of summits of the protuberances located at depth δ. As an example, Zhuravlev considered
that φ(ξ) is linear. In this case, it follows from Equation (8) that A ∼ P10/11 .
Kragelsky [23] modified the Zhuravlev approach by modelling a rough surface as a collection of
elastic flat ended rods of various heights based on a flat rigid surface. He noted that one would need
to employ the numerical integration of general expressions, if the Gaussian distribution of rod heights
were employed. Although Zhuravlev’s statistical multi-level model of surface roughness is rarely
cited, it was very successful (see [24] for further details). Indeed, the model was reborn and developed
further as the Greenwood and Williamson (GW) model. Greenwood and Williamson [25] noted that,
in the framework of the Hertz contact theory, contact between two spherical elastic solids is equivalent
to contact between a sphere of an effective radius and a plane; therefore, they do not consider contact
between two spherical asperities but rather contact between a spherical elastic asperity and a rigid
plane. Contrary to Zhuravlev, they put the origin of the vertical coordinate not at the maximum height,
but rather they took the mean plane of summit height as the reference.
As advantages of the GW model, Greenwood [26] noted the following two points: it improves on
the Zhuravlev model by assuming a Gaussian height distribution (still of identical spherical caps) and
it considers not only elastic asperities, but also plastic deformation of asperities. However, the former
advantage may be rather illusive at nanoscale. Indeed, modern nanotechnology considers surfaces
whose roughness is below the micrometre scale, while plasticity effects for crystalline materials may be
observed only at the micrometre scale and they do not arise at atomic and nanometre scales due to the
Polonsky–Keer effect. One of the authors (FB) has introduced this notation for the effect to recognize
the contribution of Polonsky and Keer [27,28] who noted first that, if the contact region of a crystalline
asperity is below some characteristic size of the microstructural length, the number of dislocations is
not large enough to cause plastic flow. This effect can be formulated as follows: ”plastic deformation
at an asperity micro-contact becomes difficult and then impossible when the asperity size decreases
below a certain threshold value on the order of the microstructural length”. Hence, in crystalline solids,
the plastic deformations of asperities may appear only within microscale asperities or at larger scales
while nanoscale asperities deform elastically (see a discussion in [29]). Furthermore, as it has been
mentioned above, the Gaussian height distribution is not observed for grinding surfaces either at micro
or nanoscales [21]. As it will be shown below, this distribution may be observed on intact surfaces. A
specific feature of the GW approach is the introduction of an exponential height distribution of the
Coatings 2018, 8, 350 6 of 17

asperity summits that allowed them to show that the true contact area A is proportional to the applied
compressive load P.
We have to add that it is a difficult task to transfer from the characteristics of a profile (or several
profiles) to the characteristics of a surface [15]—for example, to transfer the density of peaks of a
surface profile ηp to the density of asperity summits per unit area ηs of the nominally flat surface.
If φ(z) is Gaussian, then
2π
ηs = √ η2p ≈ 1.209η2p .
3 3
If the distribution of the summit height zs is Gaussian with a standard deviation σs , i.e., it is
characterized by the normalized distribution function (φs )n

z2
 
1
(φs )n = √ exp − s2 , (9)
2πσs 2σs

then the GW model is specified by three parameters: the effective radius of asperity R, the density of
asperity summits per unit area ηs and the standard deviation of the summit heights σs . It is worth
commenting that these parameters are not independent, but rather they should be related by the
equation [14,15]:
σs ηs R = const.

2.1.2. Adhesive Contact between Rough Elastic Solids

Johnson [30] presented the first model of adhesive contact between rough surfaces. Although
Johnson mentioned both Zhuravlev [22] and Greenwood and Williamson [25] models, he decided
to use the exponential distribution of summit heights of the GW model. Independently, Fuller and
Tabor [3] introduced the FT model (see also [31]). They studied the adhesive contact between rough
surfaces whose asperity heights follow the Gaussian distribution. In fact, the above models are
extensions of the GW model to the case of adhesive contact of independent spherical asperities. The
FT model is discussed in detail in [15]. This and similar models are still very popular. The statistical
approaches employed by many international teams involved in the recent competition “Contact
Mechanics Challenge” (see [32]) were based either on the use of the random process techniques applied
to the surface roughness (e.g., the auto-correlation function) or some integral parameters of the surface
roughness, e.g., the root mean square and the asperity radius of curvature.
It is worth mentioning that fractal approach to contact problems for rough surfaces was quite
popular some time ago (see a review by Borodich [33]). However, Borodich has introduced some
models that showed that fractal dimension of surfaces alone cannot characterize contact properties of
surfaces. These models include the Cantor–Borodich profile also known as the Cantor set model [34],
multi-level hierarchical model [35,36] and indenters having parametric-homogeneous (PH) profiles
[37,38]. The theory of parametric-homogeneous functions developed by Borodich is discussed in detail
in his papers [39,40].
Let us discuss two models of adhesive contact between rough surfaces introduced by Galanov
[11]. The Galanov models of contact between rough solids represent the surface roughness as a layer
whose mechanical properties differ from the bulk properties of the material (see also [41]).
It is argued in the first model that the adhesive properties of rough surfaces may be defined just by
introducing the specific work of adhesion wrough that can be written in the following dimensionless form:

∗
wrough
wrough = , (10)
σs ηs Pc

where Pc is the adhesion force, i.e., the pull–off force for a single asperity. According to the
Johnson–Kendall–Roberts (JKR) contact theory, Pc = 1.5 πwR, where w is the specific work of adhesion
of contacting pair of materials and R is the effective radius of contacting asperities.
Coatings 2018, 8, 350 7 of 17

In the refined model, the roughness is simulated as a spring mattress whose springs have nonlinear
force-displacement diagram and they stick to the opposite surface. Non-adhesive contact problems
for such layer were discussed by many authors (see, e.g., [42]). In the linear case, this layer is the
Winkler–Fuss elastic foundation that may stick to the surface. It is well known that the leading terms
of relations for the problem of contact between a compressible thin layer and a blunt punch may be
treated as a problem for the Winkler–Fuss elastic foundation; it is also possible to solve the appropriate
adhesive contact problem (see, e.g., [43]).
Furthermore, we will employ the former model of adhesive contact [11]. As many other models of
adhesive contact, this model employs implicitly the Derjaguin approximation (see a discussion in [44])
and therefore the interaction energy per unit area between small elements of curved surfaces is the
same as the interaction energy per unit area between two parallel infinite planar surfaces.
For this Galanov model, the specific work of adhesion wrough is defined as work spend for
separation of a unit area of the punch from the rough surface (see Figure 1) where P denoted the force,
p is the nominal contact pressure, P∗ = P/( NPc ) and p∗ = p/(ηs Pc ) are the dimensionless force and
pressure, and N is the number of asperities in contact. It is assumed that one can specify the distance t a
between the conventional boundary of adhesive interactions and the horizontal axis. In this case, if ∆
is the change of the spring length of the rough layer, then the distance d between the smooth plane and
the horizontal axis is defined as d = ta − ∆. This distance can be normalized by the standard deviation
d∗ = d/σ.

P* P NPc ,
* For classic unilateral
p p s Pc contact problem

0
d 0* *
wrough d* z*

Figure 1. The force-distance scheme for the classic unilateral contact and adhesive contact with a rough
surface. The area of the grey-coloured zone is equal to the specific work of adhesion wrough .

Contrary to unilateral contact, displacements of the probe may be both positive (compression)
and negative (material of the sample follow the probe due to sticking to the probe). Hence, we need
to introduce several parameters to describe adhesive contact. In addition to Pc , we need to specify δc
as the absolute value of a minimum of an asperity displacement and its normalized value δc∗ = δc /σ.
The latter value is defined according to the JKR theory as
1/3
3π2 w2 R

4 ∗
δc∗ = , K= E .
4K2 σ3 3

The effective contact modulus is E∗ = 69 · 103 Pa for the polydimethylsiloxane and epoxy resin
replicas used in [5]. Then, one can estimate the specific work of adhesion using the JKR theory and
experiments for smooth surface: w = 0.403 N/m (methods of experimental extraction w are discussed
in [8,45]).
According to the above definition, we can write
Z ∞
∗
wrough =− p∗ (z∗ )dz∗ . (11)
d0∗
Coatings 2018, 8, 350 8 of 17

Here, d0∗ is the root of the nonlinear equation

p∗ (z∗ ) = 0, (12)

i.e., p∗ (d0∗ ) = 0, while the function p∗ (z∗ ) is defined for a specified δc∗ = δc /σ as (see (4.334) in [15])
Z ∞
δ∗
 
1 h i
∗ ∗
p (z ) = √ g exp − (δ∗ + d∗ )2 dδ∗ . (13)
2π −dc∗ δc∗
∗
Thus, Equations (11)–(13) provide the full system of equations for calculation of wrough for any
∗
value of δc .
To employ the above model, one needs to extract from the experiments σ, R, and w, and calculate
ηs and the value σs ηs R. According to [15], 0.03 < σs ηs R < 0.05.

3. Statistical Analysis of Experimental Surface Topography Data

As it has been mentioned, the measurements of surface topography have been fulfilled by white
light interferometry. We need to note that only data obtained for test surfaces with nominal asperity
size 0.3 and 1 µm was good for statistical analysis. The data obtained for surfaces with higher nominal
asperity sizes were good enough only for very small domains that were separated by domains with no
proper data obtained by the interferometer. Indeed, one can see in Figure 2 that there are domains
where the white light interferometer was not able to provide proper data.

Figure 2. An example of the roughness image for surfaces with high nominal values of an asperity size
(the nominal asperity size is 9 µm). The white light interferometry was not able to provide data for
considerable number of points.

3.1. Normality Tests

As it has been shown above (see also a review in [21]), the crucial assumption of many models
of contact is that the surface roughness is Gaussian. Hence, it is important to check if the height
distribution of the tested surfaces follow the normal distribution. A large number of methods for
testing for normality [46] has been developed. Each normality test is based on a particular test
statistic that is used to give a quantitative estimation of proximity between an observed sample of
measurements and the theoretical normal distribution. The assumption of normality is especially
critical when characteristics of roughness profiles are derived. The main methods for testing for
normality are the following tests: Kolmogorov–Smirnov (KS), Lilliefors (LF), Shapiro–Wilk (SW),
Anderson–Darling (AD), Cramer–von Mises (CVM), the Pearson, and Shapiro–Francia (SF). Using
the test statistic, each of the above tests produces a numerical characteristic that is called the p-value.
Coatings 2018, 8, 350 9 of 17

This number characterizes the significance at the scale [0, 1] that the hypothesis of the normality is true
for the observed measurements. One can nominate the acceptable significance level, say 5%. If the
p-value is less than this level, then the hypothesis of normality should be rejected. Alternatively, if the
number is within the significance level, then one can conclude that the height distribution is normal.
Note that the acceptable significance level is a probability to reject the hypothesis of normality even if
it is true.
To describe the tests, we introduce notations: z(1) , . . . , z(n) is a permutation of the sample z1 , . . . , zn
such that z(1) ≤ . . . ≤ z(n) , p(i) = Φ((z(i) − z̄)/s), where Φ is the cumulative distribution function of
the standard normal distribution, and z̄ and σs are mean and standard deviation of the sample.

3.1.1. The KS Test

The Kolmogorov–Smirnov (KS) test for a sample is based on comparison of an empirical
distribution function (edf) FN (t) and the theoretical cumulative distribution function (cdf) F (t) of the
test distribution; specifically, the test statistic is
 
T = max F (z) − FN (z),
 
z

where F (z) is the cdf of Gaussian (normal) distribution and


0,

 z < z (1) ,
FN (z) = i/n, z(i) ≤ z < z(i+1) , i = 1, . . . , n − 1,


1, z ≥ z(n) ,

is the edf of the sample (z1 , z2 , . . . , z N ).

A limitation of the KS test is its high sensitivity to extreme values.

3.1.2. The LF Test

The Lilliefors (LF) test is a correction of the KS test in a way to be more conservative.
The test statistic is the maximal absolute difference between the empirical and theoretical cdf as
D = max{ D + , D − }, where

D + = max (i/n − p(i) ), D − = max ( p(i) − (i − 1)/n).

i =1,...,n i =1,...,n

The LF test is slightly better than the KS test because the LF test is more conservative.

3.1.3. The AD Test

The Anderson–Darling (AD) test is based on a squared difference between the edf and theoretical
cdf, and the test statistic is
!
1 n
Z = (1 + 0.75/n + 2.25/n ) −n − ∑ (2i − 1)(ln( p(i) ) + ln(1 − p(n−i+1) )) .
2
n i =1

The Anderson–Darling test is sensitive to discrepancies in the tails of the distribution.

3.1.4. The CVM Test

The Cramer–von Mises (CVM) test is also based on a squared difference between the edf and
theoretical cdf. The test statistic is
 !
1 n 
2i − 1 2
12n i∑
W = (1 + 0.5/n) + p (i ) − .
=1
2n
Coatings 2018, 8, 350 10 of 17

The CVM test is uniform to discrepancies in different parts of the distribution.

3.1.5. The SW Test

The Shapiro–Wilk (SW, or Shapiro) test is based on the correlation between the data and the
corresponding normal scores

(∑in=1 ci z(i) )2 m
W= n , ci = n i 2 ,
∑i=1 (z(i) − z̄) 2
∑ j =1 m j

where mi = Φ−1 ((i − 3/8)/(n + 1/4)). The Shapiro–Wilk test has better power than the KS test and
the LF test. The Shapiro–Wilk test is known as the best choice for testing the normality of data.

3.1.6. The Pearson Test

The Pearson chi-square test is based on creating the classes built in such a way that they are
equiprobable under the hypothesis of normality, where the number of classes is chosen as m = 2n2/5 .
The Pearson statistic is given by
m
P= ∑ (Cj − Ej )2 /Ej ,
j =1

where Cj is the number of counted observations and Ej is the number of expected observations under
the hypothesis of normality in the j-th class.

3.1.7. The SF Test

The Shapiro–Francia (SF) test is simply the squared correlation between the ordered sample values
and the (approximated) expected ordered quantiles from the standard normal distribution, and the
test statistic is

(∑in=1 µi z(i) )2
F= ,
∑in=1 (z(i) − z̄)2

where µi are standard normal ordered statistics.

3.2. Results of the Normality Testing

In Figure 3, we show the roughness analysis for data of the tested surface with nominal asperity
size 0.3 µm obtained by white light interferometer. The original profile measurements are given by a
black curve. A waviness is shown by a red curve. The profile measurements with removed waviness
are given by a blue curve. The height distribution for the original profile is depicted by a histogram on
the left and for the profile with removed waviness on the right.
In Figure 4, we show the statistical analysis for roughness data of the tested surface with nominal
asperity size 1 µm. The meaning of notations is the same as in Figure 3.
Several tests for normality show that the height distribution is normal. One can observe that
almost all p-values are greater that 0.05 and therefore we accept the hypothesis of normality for these
measurements. Because, as it has been shown above, the surfaces with nominal asperity size 0.3 and
1 µm do follow the Gaussian height distribution, it will be assumed further that the surfaces with
higher nominal asperity sizes follow the same distribution.
Thus, we have confirmed normality of the height distribution of these intact surfaces of the
replicas, i.e., the assumption of normality used by the above mentioned GW, FT and Galanov models
of contact between rough surface was not violated for these surfaces. Hence, these models can be used
for studies of the DSI tests of replicas of the intact surfaces of polishing paper.
Coatings 2018, 8, 350 11 of 17

spurr_0.3_1, y=109 spurr_0.3_1, y=224

1.0

Shapiro test, p=0.401, normal KS test, p=0.129, normal Shapiro test, p=0.007, not normal KS test, p=0.506, normal

1
AD test 0.185, CVM test 0.186, Lillie test 0.262, Pearson test 0.26, SF test 0.291 AD test 0.004, CVM test 0.006, Lillie test 0.006, Pearson test 0.173, SF test 0.007
0.0

0
z/ µ m

z/ µ m
−1.0

−1
AD test 0.137, CVM test 0.115, Lillie test 0.438, Pearson test 0.26, SF test 0.261 AD test 0.162, CVM test 0.265, Lillie test 0.547, Pearson test 0.388, SF test 0.05

−2
−2.0

Shapiro test, p=0.35, normal KS test, p=0.24, normal Shapiro test, p=0.062, normal KS test, p=0.811, normal
x/mm x/mm
0.00 0.05 0.10 0.00 0.05 0.10

spurr_0.3_1, y=374 spurr_0.3_2, y=109

3
1.0

Shapiro test, p=0.107, normal KS test, p=0.859, normal Shapiro test, p=0.002, not normal KS test, p=0.419, normal
AD test 0.276, CVM test 0.243, Lillie test 0.476, Pearson test 0.062, SF test 0.04

2
AD test 0.012, CVM test 0.06, Lillie test 0.11, Pearson test 0.003, SF test 0.009

1
0.0
z/ µ m

z/ µ m
0
−1.0

−2
AD test 0.124, CVM test 0.15, Lillie test 0.099, Pearson test 0.26, SF test 0.02 AD test 0.696, CVM test 0.7, Lillie test 0.76, Pearson test 0.295, SF test 0.806
−2.0

Shapiro test, p=0.054, normal KS test, p=0.474, normal Shapiro test, p=0.751, normal KS test, p=0.58, normal

−4
x/mm x/mm
0.00 0.05 0.10 0.00 0.05 0.10

spurr_0.3_2, y=224 spurr_0.3_2, y=374

3

2
Shapiro test, p=0, not normal KS test, p=0.065, normal Shapiro test, p=0, not normal KS test, p=0.227, normal
2

AD test 0, CVM test 0, Lillie test 0, Pearson test 0, SF test 0.001 AD test 0.001, CVM test 0.012, Lillie test 0.004, Pearson test 0.003, SF test 0.001

1
1

0
z/ µ m

z/ µ m
0

−1
−2

−2
AD test 0.008, CVM test 0.038, Lillie test 0.081, Pearson test 0.069, SF test 0 AD test 0.106, CVM test 0.092, Lillie test 0.097, Pearson test 0.448, SF test 0.004

−3
Shapiro test, p=0, not normal KS test, p=0.687, normal Shapiro test, p=0.009, not normal KS test, p=0.15, normal
−4

x/mm x/mm
0.00 0.05 0.10 0.00 0.05 0.10

Figure 3. Roughness data of the tested surface with nominal asperity size 0.3 µm obtained by white
light interferometer: original data (black), waviness (red) and profile with removed waviness (blue);
x-scale units are mm. The height distributions are given on the left and the right, respectively.

spurr_1_1, y=109 spurr_1_1, y=224

Shapiro test, p=0.175, normal KS test, p=0.793, normal Shapiro test, p=0.012, not normal KS test, p=0.502, normal
2
2

AD test 0.294, CVM test 0.372, Lillie test 0.541, Pearson test 0.228, SF test 0.331 AD test 0.009, CVM test 0.016, Lillie test 0.15, Pearson test 0.052, SF test 0.017
1
1

−1 0
z/ µ m

z/ µ m
−3 −2 −1 0

−2

AD test 0.038, CVM test 0.075, Lillie test 0.092, Pearson test 0.788, SF test 0.006 AD test 0.005, CVM test 0.007, Lillie test 0.134, Pearson test 0.022, SF test 0.02
−3

Shapiro test, p=0.004, not normal KS test, p=0.756, normal Shapiro test, p=0.023, not normal KS test, p=0.496, normal
x/mm x/mm
0.00 0.05 0.10 0.00 0.05 0.10

spurr_1_1, y=374 spurr_1_2, y=109

4

Shapiro test, p=0.029, not normal KS test, p=0.745, normal Shapiro test, p=0, not normal KS test, p=0.141, normal
2

AD test 0.494, CVM test 0.645, Lillie test 0.83, Pearson test 0.694, SF test 0.022 AD test 0.001, CVM test 0.001, Lillie test 0.004, Pearson test 0.209, SF test 0.001
2

1
z/ µ m

z/ µ m
−3 −2 −1 0
−2
−4 0

AD test 0.118, CVM test 0.132, Lillie test 0.255, Pearson test 0.228, SF test 0.019 AD test 0.101, CVM test 0.158, Lillie test 0.423, Pearson test 0.26, SF test 0.059
Shapiro test, p=0.042, not normal KS test, p=0.312, normal Shapiro test, p=0.108, normal KS test, p=0.63, normal
x/mm x/mm
0.00 0.05 0.10 0.00 0.05 0.10

spurr_1_2, y=224 spurr_1_2, y=374

4

Shapiro test, p=0, not normal KS test, p=0.025, not normal Shapiro test, p=0.274, normal KS test, p=0.374, normal
AD test 0, CVM test 0, Lillie test 0, Pearson test 0, SF test 0
2

AD test 0.096, CVM test 0.067, Lillie test 0.03, Pearson test 0.228, SF test 0.247
2

1
z/ µ m

z/ µ m
0
−2 0

−2

AD test 0.373, CVM test 0.377, Lillie test 0.475, Pearson test 0.095, SF test 0.59 AD test 0.008, CVM test 0.013, Lillie test 0.021, Pearson test 0.044, SF test 0.002
−4

Shapiro test, p=0.567, normal KS test, p=0.531, normal Shapiro test, p=0.004, not normal KS test, p=0.358, normal
−4

x/mm x/mm
0.00 0.05 0.10 0.00 0.05 0.10

Figure 4. Roughness data of the tested surface with nominal asperity size 1 µm. The meaning of
notations is the same as in Figure 3.

4. The Indentation Tests of Epoxy Resin Replicas and Theoretical Modelling

4.1. Experimental Data Obtained by DSI

As it has been mentioned above, the force tester Basalt 01 was used in the DSI tests. Epoxy-resin
replicas of a smooth glass surface and five rough surfaces were used as substrates. For measurements of
adhesion forces, a micro-force tester equipped with a double-leaf spring serving as a cantilever beam was
applied. Here, a soft spherical probe was pressed with a given force onto a sample. The required force to
release the probe from the surface (pull-off force) corresponds to the adhesive property of the sample.
Coatings 2018, 8, 350 12 of 17

If the surfaces were smooth, then, in the case of a spherical probe, the real contact area and effective elastic
modulus could be calculated according to the Johnson–Kendall–Roberts (JKR) theory, which is a well
established standard analyze method for micro-scale adhesion between elastic materials.
The JKR theory was developed for adhesive contact between two smooth elastic spheres or a
rigid sphere and an elastic half-space (see for details [1,44,47]). However, here we consider contact
interactions between relatively rigid epoxy resin replicas and a soft polydimethylsiloxane sphere.
These are polymer materials. Properties of such materials are time-dependent and their elasticity is
often described by Volterra integral equations [48]. However, if the kernel of the Volterra equation
is not singular (the physical meaning of this condition is that the rearrangements of long polymer
chains in both materials are not very fast), then, for short times for the loading–unloading tests, the
materials may be quite often treated as elastic ones. Furthermore, adhesion of polymers may have
different physical origin (see [49] and also a comprehensive review [50]). However, if the loading to
the prescribed maximal compressive force and unloading of the samples take the same short amount
of time for all samples, then it is quite convenient to use "the specific work of adhesion of contacting
pair of materials" and use these values to compare the results of the tests.
The experimental absolute value of the pull-off force for replica of smooth glass surface was
exper
Pc = 2845 µN. Absolute average values of measured pull-off forces are presented in the 4th
exper
column of Table 2. One can see that the highest average of the pull-off force value Pc = 3823 µN
was obtained not on the smooth sample, but on the rough surface whose nominal size of surface
asperities was 0.3 µm. The pull-off forces decreased continuously with the further increase of the
surface micro-roughness [5].

Table 2. The final outcomes of theoretical calculations in comparison with experimental results.

rough exper
Nominal Size of Surface Asperities (µm) wrough [N/m] Pc [mN] Pc [mN]
0.3 1.43 10.12 3.823
1 0.66 4.69 3.022
3 0.39 2.74 2.779
9 0.31 2.18 2.251
12 0.29 2.03 2.108

4.1.1. Modelling of Surfaces as Random Process Graphs

Here, we will provide some theoretical justifications of the plausible explanation of the
experimental data given in [5].
First, we note that the greater the area of the true contact, the stronger the adhesion absolutely
irrespective to the nature and the value of the forces carrying out the adhesive connection [51].
Assuming that there is almost full contact between the smooth spherical probe and the tested surface
for both the nominally flat sample and the surface having the nominal asperity size of 0.3 µm, one can
estimate the full area of the rough surface.
Of course the Galanov model has the same limitations as the Zhuravlev, GW, and FT models of
discrete contact: it is assumed that contacts between asperities do not influence each other. Hence,
if the rough surface of the nominal asperity size of 0.3 µm has full contact with the probe, then the
model cannot be applied. Let us estimate the total area of the rough surface.
Khusu et al. [13] studied several correlation functions for rough profiles having Gaussian height
distributions. The asperity heights were calculated from the middle line of the profile, that, in turn,
was calculated by the least square method. This was leading to introduction of additional parameters.
Using this description, Linnik and Khusu [20] measured various parameters. In particular, they studied
(i) the fraction of the horizontal line at a specific level, which lies within the roughness profile, i.e., they
calculated the Abbott–Firestone curve, and (ii) the total area of the profile curve above this horizontal
line. They reported pretty good agreement of the obtained results with their particular experimental
observations. They suggested also to use the Abbe test for checking that the expectations of all values
Coatings 2018, 8, 350 13 of 17

are the same, i.e., there are no trends in data. In addition to K ( x ) of form in Equation (5), which is
a correlation function of a homogeneous isotropic random field, they also studied the correlation
function
2 2
K2 ( x ) = K2 (0) · e−α2 x , (14)

where K2 (0) and α2 are some parameters of the roughness. The correlation functions given by
Formulas (5) and (14) will be used here to estimate the true area of rough surfaces.
From the real data of roughness over the rectangular (0.11 mm × 0.14 mm), we compute the
number of summits N and the number of summits per unit area ηs . Taking σs ηs R = 0.035, one can
calculate the radius of curvature of an asperity as R = 0.035/(σs ηs ). The results of calculations are
presented in Table 3.
The calculations were fulfilled in the following steps.

Table 3. The parameters of the Galanov model.

Nominal Size of Surface Asperities (µm) N ηs [m−2 ] R (µm) δc (m) Padh [N] δ∗
0.3 1975 12.82 · 1010 1.33 5.73 · 10−6 2.52 · 10−6 27.98
1 1213 7.87 · 1010 0.79 4.83 · 10−6 1.51 · 10−6 8.62
3 153 0.997 · 1010 2.06 6.64 · 10−6 3.92 · 10−6 3.90
9 10.8 0.07 · 1010 12.08 12.2 · 10−6 24.3 · 10−6 3.13
12 8.2 0.053 · 1010 15.0 12.9 · 10−6 28.4 · 10−6 2.92

Using the values of δ∗ obtained, we calculated the values of wrough

∗ by Equations (11)–(13) of the
∗
Galanov model. Finally, we compute the specific adhesion work of rough surface wrough = σηs Pc wrough
and the real force of adhesion between a smooth sphere (probe) of radius Rs = 1.5 mm and rough
rough ∗
surface as Pc = 1.5πRs wrough .
exper
The 4th column of Table 2 shows the average of the experimental pull-off force Pc [5]. These
experimental values are close to the adhesion force given in the 3rd column calculated for contact
between a smooth spherical probe of radius Rs = 1.5 mm and rough surface when the surface has
rough
nominal size of asperities larger or equal to 3 µm. However, the calculated values Pc are not close
to the experimental values for surfaces with nominal size 0.3 µm and 1 µm because there exists almost
full contact and the Galanov model along with the FT or GW models are not applicable.
In the case of full contact, it is useful to compare the true area of the rough surface and the
smooth one.
The length of a realization of a random Gaussian process z( x ) on a unite interval is
Z L
1
s= [1 + z02 ( x )]1/2 dx.
L 0

If the standard deviation of the process σ/L << 1 and one employs the correlation function given
by Equation (14), then one can write an asymptotic series for its expectation Es (see Chapter 2.9 in [13]).
It follows from Table 1 that rough profile having nominal asperity height 0.3 µm has σ = 0.205 µm over
an interval L = 140 µm, i.e., σ/L = 0.205/140 << 1. Hence, the asymptotic series may be used. One
can get that the estimations of the profile length are very small in the case if the correlation function
given by Equation (14) is employed. We can conclude that Equation (14) does not reflect the horizontal
distribution of asperities. However, our computations using numerical simulations of a Gaussian
process with the exponential correlation function given by Equation (5) show that the length of the
profile increases. Simulating the surface with the nominal size of asperities 0.3 µm and computing
the length of profiles along several lines, we have obtained that s/L = 1.16. If we estimate the ratio
of the true area of the rough surface to the nominal area as Atrue /Anominal = (s/L)2 , then we obtain
exper
Atrue /Anominal = 1.162 = 1.3456. On the other hand, the ratio of Pc for the surface with nominal
asperity heights 0.3 µm to the pull-off force for the smooth one is 3.823/2.845 = 1.3438. These ratios
Coatings 2018, 8, 350 14 of 17

are in excellent agreement between each other. Thus, the plausible explanation of the observations
given in [5] are correct and supported here by our theoretical considerations.

5. Conclusions
Currently, the design of many devices is influenced by discoveries of structures of biological
objects. It is known that attachment organs of insects have worse performance at surfaces having
specific roughness and this idea is used in preparation of the so-called anti-adhesive materials. To study
effects of surface roughness on molecular adhesion between solids, it was suggested earlier to prepare
epoxy resin replicas of surfaces having different roughness and conduct contact loading tests of the
samples using a micro-force tester with a spherical smooth probe. Because the materials of all samples
are the same, the roughness effects are not influenced by other factors. The contact loading tests
between different samples showed a rather surprising results: a surface having very small roughness
showed the greater values of the force of adhesion than the replica of a smooth surface. A plausible
explanation of the observations was given in [5], suggesting that these rough surfaces had full adhesive
contact while their true contact area is greater than the area for a smooth surface, and the surfaces with
higher values of roughness do not have full contact.
One of the main purposes of the paper is to justify theoretically these explanations. Evidently,
one needs to use a theory of adhesive contact between rough surfaces. Unfortunately, the main theories
of contact between rough surfaces were developed for roughness whose height distributions are
Gaussian. However, one cannot assume that the surfaces always have normal (Gaussian) roughness.
For example, it was shown that the grinding surfaces are not Gaussian either at micro or nanoscale [21].
To check the assumption that the roughness is Gaussian, various modern tests of normality of data
have been employed. These tests include the Kolmogorov–Smirnov, Lilliefors, Shapiro–Wilk, Pearson,
Anderson–Darling, Cramer–von Mises and Shapiro–Francia ones. Of course, there are many other
tests of normality (see a discussion in [46]). However, the tests used are the most popular ones. These
tests showed that the height distribution of the surfaces under investigation are normal (Gaussian).
We can conclude that, for replicas of polishing papers, the exponential correlation function given
by Formula (5) may be used to model horizontal distribution of asperities having Gaussian vertical
distribution. The polydimethylsiloxane sphere is soft enough material to provide full contact for
the surface with nominal asperity heights 0.3 µm, while, for the used load, the full contact was
not observed for surfaces having higher roughness. Using one of the Galanov models of adhesive
contact between rough surfaces, the experimental observations are explained for surfaces whose
nominal asperity values were over 1 µm. For a surface with nominal asperity heights 0.3 µm, we have
provided the results of numerical simulations of random surfaces and justified the above explanations
using geometrical arguments. Thus, the plausible explanation of observations have been theoretically
justified.

Author Contributions: Conceptualization, A.P., F.M.B. and S.N.G.; Methodology, A.P., F.M.B., E.V.G. and S.N.G.;
Software, A.P.; Formal Analysis, A.P., B.A.G. and F.M.B.; Investigation, E.V.G and S.N.G.; Resources, S.N.G and
E.V.G.; Data Curation, A.P. and S.N.G.; Writing-Original Draft Preparation, F.M.B.; Visualization, A.P.
Funding: This research received no external funding.
Acknowledgments: The collaboration of the authors on the topic of the paper was initiated within the CARBTRIB
International network. The authors are grateful to the Leverhulme Trust for support of the CARBTRIB Network.
The study was fulfilled during the stay of one of the authors (F.M.B.) at the Functional Morphology and
Biomechanics group (University of Kiel). F.M.B. is grateful to Alexander von Humboldt Foundation for financial
support of the research visit.
Conflicts of Interest: The authors declare no conflict of interest.
Coatings 2018, 8, 350 15 of 17

References
1. Kendall, K. Molecular Adhesion and Its Applications; Kluwer Academic/Plenum Publishers: New York, NY,
USA, 2001.
2. Eichler-Volf, A.; Kovalev, A.; Wedeking, T.; Gorb, E.V.; Xue, L.; You, C.; Piehler, J.; Gorb. S.N.; Steinhart. M.
Bioinspired monolithic polymer microsphere arrays as generically anti-adhesive surfaces. Bioinspir. Biomim.
2016, 11, 025002. [CrossRef] [PubMed]
3. Fuller, K.N.G.; Tabor, D. The effect of surface roughness on the adhesion of elastic solids. Proc. R. Soc. Lond. A
1975, 345, 327–342. [CrossRef]
4. Gorb, E.; Haas, K.; Henrich, A.; Enders, S.; Barbakadze, N.; Gorb, S. Composite structure of the crystalline
epicuticular wax layer of the slippery zone in the pitchers of the carnivorous plant Nepenthes alata and its
effect on insect attachment. J. Exp. Biol. 2005, 208, 4651–4662. [CrossRef] [PubMed]
5. Purtov, J.; Gorb, E.V.; Steinhart, M.; Gorb, S.N. Measuring of the hardly measurable: adhesion properties of
anti-adhesive surfaces. Appl. Phys. A 2013, 111, 183–189. [CrossRef]
6. Gorb, E.; Purtov, J.; Gorb, S. Adhesion force measurements on the two wax layers of the waxy zone in
Nepenthes alata pitchers. Sci. Rep. 2014, 4, 5154. [CrossRef] [PubMed]
7. Borodich, F.M.; Galanov, B.A.; Gorb, S.N.; Prostov, M.I.; Prostov, Y.I.; Suarez-Alvarez, M.M. Evaluation of
adhesive and elastic properties of materials by depth-sensing indentation of spheres. Appl. Phys. A Mater.
Sci. Process. 2012, 108, 13–18. [CrossRef]
8. Borodich, F.M.; Galanov, B.A.; Gorb, S.N.; Prostov, M.Y.; Prostov, Y.I.; Suarez-Alvarez, M.M. Evaluation of
adhesive and elastic properties of polymers by the BG Method. Macromol. React. Eng. 2013, 7, 555–563.
[CrossRef]
9. Jiao, Y.; Gorb, S.; Scherge, M. Adhesion measured on the attachment pads of Tettigonia viridissima (Orthoptera,
insecta). J. Exp. Biol. 2000, 203, 1887–1895. [PubMed]
10. Perepelkin, N.V.; Kovalev, A.E.; Gorb, S.N.; Borodich, F.M. Estimation of the elastic modulus and the work of
adhesion of soft materials using the extended Borodich-Galanov (BG) method and depth sensing indentation.
Mech. Mater. 2018, in press.
11. Galanov, B.A. Models of adhesive contact between rough elastic bodies. Int. J. Mech. Sci. 2011, 53, 968–977.
[CrossRef]
12. Goryacheva, I.G. Contact Mechanics in Tribology; Kluwer: Dordreht, The Nederlands, 1997.
13. Khusu, A.P.; Vitenberg, Y.R.; Palmov, V.A. Roughness of Surfaces: Theoretical Probabilistic Approach; Nauka:
Moscow, Russia, 1975.
14. Whitehouse, D.J.; Archard, J.F. The properties of random surfaces of significance in their contact.
Proc. R. Soc. Lond. 1970, 316, 97–121. [CrossRef]
15. Maugis, D. Contact, Adhesion and Rupture of Elastic Solids; Springer-Verlag: Berlin, Germany, 2000.
16. Nowicki, B. Multiparameter representation of surface roughness. Wear 1985, 102, 161–176. [CrossRef]
17. Whitehouse, D.J. The parameter rash—Is there a cure? Wear 1982, 83, 75–78. [CrossRef]
18. Abbott, E.J.; Firestone, F.A. Specifying surface quality: A method based on accurate measurement and
comparison. Mech. Eng. 1933, 55, 569–572.
19. Meetings of the Town’s Mathematical Seminar in Leningrad. Uspekhi Mat. Nauk 1954, 9, 255–256. (In Russian)
20. Linnik, Y.V.; Khusu, A.P. Mathematical and statistical description of unevenness of surface profile at grinding.
Bull. USSR Acad. Sci. Div. Tech. Sci. 1954, 20, 154–159. (In Russian)
21. Borodich F.M.; Pepelyshev, A.; Savencu, O. Statistical approaches to description of rough engineering
surfaces at nano and microscales. Tribol. Int. 2016, 103, 197–207. [CrossRef]
22. Zhuravlev, V.A. On question of theoretical justification of the Amontons-Coulomb law for friction of
unlubricated surfaces. Proc. Inst. Mech. Eng. Part J J. Eng. Tribol. 2007 221, 894–898. [CrossRef]
23. Kragelsky, I.V. Static friction between two rough surfaces. Bull. USSR Acad. Sci. Div. Tech. Sci. 1948, 10,
1621–1625. (in Russian)
24. Borodich, F.M. Translation of Historical Paper. Introduction to V A Zhuravlev’s historical paper: ‘On the
question of theoretical justification of the Amontons-Coulomb law for friction of unlubricated surfaces’.
Proc. Inst. Mech. Eng. Part J J. Eng. Tribol. 2007, 221, 893–898.
Coatings 2018, 8, 350 16 of 17

25. Greenwood, J.A.; Williamson, J.B.P. Contact of nominally flat surfaces. Proc. R. Soc. Lond. A 1966, 370, 300–319.
[CrossRef]
26. Greenwood, J.A. Surface modelling in tribology. In Applied Surface Modelling; Creasy, C.F.M., Craggs, C., Eds.;
Ellis Horwood: New York, NY, USA, 1990; pp. 61–75.
27. Polonsky, I.A.; Keer, L.M. Scale effects of elastic-plastic behavior of microscopic asperity contacts. J. Tribol.
Trans. ASME 1996, 118, 335–340. [CrossRef]
28. Polonsky, I.A.; Keer, L.M. Simulation of microscopic elastic-plastic contacts by using discrete dislocations.
Proc. R. Soc. A 1996, 452, 2173–2194. [CrossRef]
29. Borodich F.M.; Savencu, O. Hierarchical models of engineering rough surfaces and bioinspired adhesives.
In Bio-Inspired Structured Adhesives; Heepe, L., Gorb, S., Xue, L., Eds.; Springer: Berlin, Germany, 2017.
30. Johnson, K.L. Non-Hertzian contact of elastic spheres. The mechanics of the contact between deformable
bodies. In Proceedings of the IUTAM Symposium ; De Pater, A.D., Kalker, J.J., Eds.; Delft University Press: Delft,
The Nederland, 1975; pp. 26–40.
31. Fuller, K. Effect of surface roughness on the adhesion of elastomers to hard surfaces. Mater. Sci. Forum
2011, 662, 39–51. [CrossRef]
32. Carpick, R.W. The contact sport of rough surfaces. Science 2018, 359, 38. [CrossRef] [PubMed]
33. Borodich, F.M. Fractal Contact Mechanics. In Encyclopedia of Tribology; Wang, Q.J., Chung, Y.-W., Eds.;
Springer: Berlin, Germany, 2013; Volume 2, pp. 1249–1258.
34. Borodich, F.M.; Mosolov, A.B. Fractal roughness in contact problems. PMM J. Appl. Math. Mech. 1992, 56,
681–690. [CrossRef]
35. Borodich, F.M.; Onishchenko, D.A. Fractal roughness for problem of contact and friction (the simplest
models). J. Frict. Wear 1993 14, 452–459.
36. Borodich, F.M.; Onishchenko, D.A. Similarity and fractality in the modelling of roughness by a multilevel
profile with hierarchical structure. Int. J. Solids Struct. 1999, 36, 2585–2612. [CrossRef]
37. Borodich, F.M. Similarity properties of discrete contact between a fractal punch and an elastic medium.
Comptes Rendus L’Académie Sci. 1993, 316, 281–286.
38. Borodich, F.M.; Galanov, B.A. Self-similar problems of elastic contact for non-convex punches. J. Mech.
Phys. Solids 2002, 50, 2441–2461. [CrossRef]
39. Borodich, F.M. Parametric homogeneity and non-classical self-similarity. I. Mathematical background.
Acta Mech. 1998, 131, 27–45. [CrossRef]
40. Borodich, F.M. Parametric homogeneity and non-classical self-similarity. II. Some applications. Acta Mech.
1998, 131, 47–67. [CrossRef]
41. Galanov, B.A.; Valeeva, I.K. Sliding adhesive contact of elastic solids with stochastic roughness. Int. J.
Eng. Sci. 2016, 101, 64–80. [CrossRef]
42. Galanov, B.A. Spatial contact problems for rough elastic bodies under elastoplastic deformations of the
unevenness. PMM J. Appl. Math. Mech. 1984, 48, 750–757. [CrossRef]
43. Borodich, F.M.; Galanov, B.A.; Perepelkin, N.V.; Prikazchikov, D.A. Adhesive contact problems for a thin elastic
layer: Asymptotic analysis and the JKR theory. Math. Mech. Solids 2018. [CrossRef]
44. Borodich, F.M. The Hertz-type and adhesive contact problems for depth-sensing indentation. Adv. Appl.
Mech. 2014, 47, 225–366.
45. Borodich, F.M.; Galanov, B.A. Non-direct estimations of adhesive and elastic properties of materials by
depth-sensing indentation. Proc. R. Soc. A 2008, 464, 2759–2776 . [CrossRef]
46. Thode, H.C. Testing for Normality; Marcel Dekker: New York, NY, USA, 2002.
47. Johnson, K.L.; Kendall, K.; Roberts, A.D. Surface energy and the contact of elastic solids. Proc. R. Soc. Lond. A
1971, 324, 301–313. [CrossRef]
48. Rabotnov, Y.N. Elements of Hereditary Solid Mechanics; Mir Publishers: Moscow, Russia, 1980.
49. Kovalev, A.; Sturm, H. Polymer Adhesion. In Encyclopedia of Tribology; Wang, Q.J., Chung, Y.-W., Eds.;
Springer: Berlin, Germany, 2013; pp. 2551–2556.
50. Myshkin, N.; Kovalev, A. Adhesion and surface forces in polymer tribology—A review. Friction 2018, 6,
143–155. [CrossRef]
Coatings 2018, 8, 350 17 of 17

51. Derjaguin, B.V.; Krotova, N.A.; Smilga, V.P. Adhesion of Solids; Consultants Bureau: New York, NY, USA, 1978.

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