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i
Abstract
Inspired from microstructure-based reversible fastening mechanisms in
biological system, a number of researches have been conducted to elucidate
the principle of adhesion and to mimic its function. Structures with high
aspect ratio have been desirably used to maximize van der Waals force,
though the weakness of the structures has been one of the major huddles for
practical use. Here, instead of high aspect ratio structures which are
vulnerable to mechanical failure, the interlocking between arrays of regularly
protruded line structures is introduced to provide remarkable repeatability
while maintaining substantial adhesion force. Mechanical interlocking
between line arrays made by UV-curable material is mediated by van der
Waals interaction when two surfaces are brought into contact. By optimizing
the geometry and material, ‘failure-free’ working condition is established and
maximum measured adhesion force is recorded about ~ 29.6 N/cm2 without
any degradation in adhesion force during repeatable attachment. To analyze
the adhesion characteristics, a theoretical model is established using
Timoshenko beam bending theory and van der Waals interaction between two
surfaces with nanoscale roughness.
Keywords : biomimetics, reversible interlocking, line array
structure, dry adhesive, van der Waals force
Student Number : 2012-22563
ii
Contents
Abstract i
Nomenclature iii
List of Figures iv
1. Introduction 1
2. Experimental Results
2.1. Fabrication of PUA line arrays
2.2. Adhesion measurements
2.3. Repeatability test
5
6
9
3. Analysis
3.1. Beam deflection analysis
3.2. Van der Waals force analysis and combined modeling
12
14
4. Conclusion 17
Experimental Section
Figures
References
19
21
29
Abstract (Korean) 33
iii
Nomenclature
λ
E
𝑃𝑐
𝐼
𝐿
𝜎𝑏
𝑀𝑏
𝑦
𝑀
G
𝜈
𝜅
𝛿
𝜎
Wavelength of light
Elastic modulus (Young’s modulus)
Critical buckling load
Second moment of inertia
Height of the line structure
Bending stress of the structure
Bending moment of the structure
Distance from the neutral axis
Deflection of the beam
Bending moment of the beam
Shear modulus
Poission’s ratio
Cross-sectional area
Shear correction coefficient
Deflection length
Hamaker constant
Cut-off distance
Probability of area in contact
Surface energy
RMS roughness of the surface
Friction coefficient
Bending angle
iv
List of Figures
Figure 1. (a) Fabrication process of a PUA line array by two-step
molding method. (b) Schematic illustration of the interlocking
procedure. (c) Cross-sectional SEM image of interlocked line
array.
Figure 2. (a) SEM images of the nanoscale line array (width = 800 nm)
with three different spacing ratios (1, 3, and 5). The inset
shows bird-view of the each array. (b) Measured normal and
shear adhesion force of samples.
Figure 3. (a) SEM images of the line structure array with three different
feature sizes (400 nm, 800 nm, and 5 μm). The inset shows
bird-view of the each array. (b) Plots showing a growing
tendency of the adhesion force as pattern size increases. (c-d)
Macroscopic locking status and corresponding cross-sectional
SEM images of (c) 800 nm feature size and (d) 5um feature
size.
Figure 4. Adhesion graph showing normal and shear adhesion forces
with different materials.
Figure 5. (a) Measurement of adhesion forces with repeating cycles of
attachment and detachment up to ~250 cycles of normal
v
direction and ~100 cycles of shear direction. (b) SEM images
of a pristine line array sample and the same after normal and
shear repeatability test. (c) Two representative failure modes
of the protruded structure with different types of external
loads.
Figure 6. (a) Schematic illustration of the deflection and force
equilibrium of the interlocked structure. (b) 3-D AFM image
showing the nanoscale roughness on the surface of the pattern.
(c) Optical microscope images of the interlocked line array,
showing that locked and unlocked region is coexisted. (d)
Plots of expected shear adhesion force predicted by two types
of beam bending theories and measured adhesion force that
follows Timoshenko beam bending theory.
Figure 7. Photographs of a custom-built equipment used to measure the
normal and shear adhesion force of samples. A load cell is
installed for each direction and the pulling force is applied by
motorized moving part.
1
1. Introduction
2
Reversible fastening and fixation ability is known as one of the crucial
requirements for the survival of a number of species in nature, which can be
realized by various systems including mechanical, electrochemical, and
capillary-based principles.[1-3]
Structure-based locking apparatus has been
widely employed for various species, for example, the hook structure of the
plants,[4,5]
interlocking system of dragonfly’s head arrester[6]
and wing locking
system in beetles.[7]
Recently, a gear-like structure was found in plant hoppers,
which enables synchronized movements of each leg for the jumping process.[8]
Inspired from aforementioned biological system, there have been
many attempts to take advantage of structure-based mechanical locking
effects realized by various shapes and materials such as core-shell nanowire
forest,[9,10]
carbon nanotubes (CNTs),[11,12]
polymer nanofibers,[13,14]
sharp
particles,[15]
and rippled structure.[16-18]
In these cases, the attractive van der
Waals force plays a key role to exert stable adhesion. It has been known that
the structures with high aspect ratio (HAR) are desirably used to maximize the
van der Waals effect by providing larger surface area. A wide variety of
valid results have presented theoretical prediction.[13,19]
However, due to its intrinsic mechanical instability, HAR structures
are vulnerable to irreversible buckling, mating, and lateral collapsing when
external load is applied or the structures are contacted with each other.[20,21]
Though damaged structures of biological organisms, which consist of β-
keratin can be easily regenerated, synthetic HAR fibers cannot recover its
original shape after mechanical failures.[13,14,22]
Such unstable characteristic of
HAR structures is one of the major obstacles for a repeatable and practical
attachment system.
3
Therefore, the realization of the repeatable high adhesion system by
mechanically stable structures is highly demanded for the practical application
of dry adhesive system. Here, protruded line array structures with relatively
low AR (~2) and wide pattern provide greater structural stability than HAR
features. Based on mechanical robustness, line interlocking system shown
here exerts exceptionally high repeatability while maintaining its strong
adhesion forces both in the normal and shear direction. Also, line arrays are
easily replicated using ultraviolet (UV) curable materials that may enable
large area fabrication. In this paper, the ideal condition of interlocking with
line arrays is presented in terms of geometric and material aspects, compared
with the case of HAR fibers. Also, a theoretical model for the present system
is established using Timoshenko beam bending theory and van der Waals
interaction.
4
2. Experimental results
5
2.1. Fabrication of PUA line arrays
The entire fabrication process of line array structures by UV-curable material
is summarized in Figure 1(a). First, the silicon masters engraved with various
types of line arrays were fabricated by conventional photolithography and
deep reactive ion etching (DRIE) process. The surface of the master mold is
treated with octafluorocyclobutane (C4F8) gas in the inductively coupled
plasma (ICP) chamber for the easy detachment of polymers.
To fabricate the 1st replica, polydimethylsiloxane (PDMS) precursor
mixed with 10 wt% of curing agent (Sylgard 184, Dow Corning) was poured
onto the silicon mold. After degassing process in a vacuum chamber, it was
cured at 70℃ for 1 hour and the PDMS replica was carefully peeled off from
the silicon master mold. . This series of process can be repeated several times
to make multiple replica molds. After that, two types of PUA prepolymers (s-
PUA; PUA MINS 311 RM, h-PUA; PUA MINS 301 RM, purchased from the
Minuta Tech, Korea) were prepared for the UV molding process to make the
2nd replica. A drop of PUA was dispensed onto the master mold and a
polyethylene terephthalate (PET) film (50 μm thickness) was slightly pressed
against the liquid drop for it to be used as a supporting layer. The precursor
was exposed to UV light (λ=250-400 nm, intensity of ~100 W/cm2, Fusion
Cure System, Minuta Tech, Korea) during the curing time about ~60 seconds.
After exposure, it was detached from the PDMS mold by peeling off the
substrate, followed by additional exposure to UV light for several hours for
complete curing.
6
2.2. Adhesion measurements
Figure 1(b) shows an illustration of the interlocking procedure between as-
made line array structures, and corresponding cross-sectional image is shown
in Figure 1(c). Before initial contact, the upper and lower line array structure
samples should be aligned to secure parallel state. When the locking is
initiated at one side, sequential locking is triggered by pressing the sample
towards the other side. This line-to-line locking process is analogous to the
fastening procedure of conventional zipper in the way that complementary
structure is clasped with each other by external load.
To find out the optimal geometry of this ‘zipper-like’ contact, a series
of experiments were conducted. First, the adhesion test about line arrays with
several sets of different spacing ratio (SR, defined as line spacing/line width)
was conducted to find out which one would be the most effective condition
for interlocking phenomena. For each case, the width of individual line
structure is fixed as 800 nm (Figure 2(a)). The result shown in Figure 2(b)
indicates that in the case of SR of 3 and 5, both normal and shear adhesion
force is comparable or even less than flat-to-flat adhesion (~2.3 N/cm2 for
normal and ~8.6 N/cm2 for shear direction), whereas the significant increase
in adhesion force is observed in the case of SR=1 (~ 6.1 N/cm2 for normal and
~15.7 N/cm2 for shear). In short, smaller spacing ratio is more advantageous
because of not only larger contact surfaces but also more probability of
contact caused by the narrowed spacing between adjacent structures. This
tendency is truly distinguishable, given that interlocking between HAR hairy
structures is hard to occur for the case of SR≅1, especially attributed to the
buckling of the structure.[14]
7
Next, to find out the relationship between the pattern size and
adhesion force, adhesion tests were performed with three different samples
(Figure 3(a)). Interestingly, it is found that there is a monotonic increment in
adhesion force as the width of the line structure feature becomes larger. In the
case of HAR hairs, the contacted area of interlocked hairs is directly
proportional to the density of hair array and thus the smaller the hair feature
size, the greater the adhesion force[13]
. However, when employing the line
structure, both maximum normal (~8.5 N/cm2) and shear (~29.6 N/cm
2)
adhesion force is measured when the width of structure is 5 μm (Figure 3(b)).
This phenomenon can be explained by the difference in the macroscopic areal
fraction of interlocked region. As seen in Figure 3(c), in the case of nanoscale
line array, the complete locking region is distinguishable by naked eye since
the region becomes optically transparent as the spacing is completely filled
with the counterpart. The picture shows that fully locked region is sparsely
scattered over the entire area, which leads to the loss of adhesion force. This is
attributed to the fact that it is very tricky to align the array consisting of
nanoscale feature. The perfect alignment of nanoscale line array is beyond the
level of manual manipulation by hand. On the other hand, microscale array
shows uniform locking for the entire area (Figure 3(d)) thereby providing
stronger adhesion. One thing to note is that even for the case of SR=1, the
width of the spacing should be slightly wider than the width of the line
structure (SR of ~1.2 is used in this paper) to maintain clearance fit condition,
unless interlocking does not occur since the structures are hardly fitted into
the space.
Aside from geometrical aspects, the effect of elastic modulus of
8
building material was investigated. The elastic modulus (denoted as E) of
PUA material can be tuned by changing the component and ratio of modulator,
which has been reported in earlier reports.[23,24]
In this experiment, two types
of UV-curable materials were used: s-PUA (E=19.8 MPa) and h-PUA (E=320
MPa). The geometry of the samples is fixed as width of 800 nm and SR of 1.
The result shows that structures with s-PUA present higher adhesion force
than h-PUA structures (Figure 4), which is consistent with previous
experimental results[13]
. The reason for the higher adhesion force in softer
material can be explained in terms of the probability of conformal contact
with the nanoscale roughness, which is discussed in the following section.
9
2.3. Repeatability test
To demonstrate the durability of the interlocking system, 250 cycles and 100
cycles of the normal and shear attachment test were conducted, respectively
(Figure 5(a)). As seen, no sign of degradation in normal and shear adhesion
force is observed throughout the experiment, and the structural rigidity is also
verified by the SEM image after the test (Figure 5(b) and (c)). It is notable
that such robust adhesion is achieved without any surface modification such
as coating with metals[13,22,25]
. To elaborate the remarkable durability of line
structure compared with HAR hairs, a simple theory is introduced. For the
case of a long-term repeatable adhesion, failures of protruded structure can
happen in the form of two cases depending on the direction of external load
depicted in Figure 5(d): i) buckling of structure due to normal load, and ii)
fracture at the bottom induced by tensile bending stress.
In the case of buckling, it would happen when the paired structure is
faced each other at the top surface and squashed by pressing force. Assuming
clamped end at the bottom and hinged end at the top side, critical buckling
load (𝑃𝑐) of the single structure can be expressed as[26]
𝑃𝑐 = 20.2𝐸𝐼
𝐿2
where 𝐼 is the second moment of inertia and 𝐿 is the height of the structure,
respectively. After calculating 𝑃𝑐 of the individual unit, macroscopic critical
pressure can be calculated by considering the areal density of the array. When
considering the micro-scale line structure used in Figure 5 (width=5 μm,
SR=1, and AR=2), critical buckling pressure is estimated as 3.3 MPa (=330
10
N/cm2), which is far beyond the range of applied preload (~10 N/cm
2). But in
the case of the polymeric hairy structure, both SR and AR needs to be higher
than this value (SR of ~3 and AR of ~10[13,14,27,28]
) to raise the probability of
contact and amplify surface contact area for significant decrease in the critical
buckling pressure.
Also, bending stress should be considered to figure out whether the failure of
the structure would happen. In the case of the bending of the cantilever, the
stress caused by the applied bending moment, 𝜎𝑏, can be expressed as[26]
𝜎𝑏 =𝑀𝑏𝑦
𝐼
where 𝑀𝑏 is the bending moment at the section and 𝑦 is the distance from
the neutral axis, respectively. According to the measured shear adhesion force
and the assumption of distributed load condition, calculated average bending
stress at the bottom of the structure is about 4.5 MPa which is half of the
ultimate tensile stress of the s-PUA (~9 MPa[23]
).
Consequently, the failure of the whole line structure is hardly expected during
the regular attachment and detachment process, except for gradual surface
abrasion due to sliding between contact surfaces.
11
3. Analysis
12
3.1. Beam deflection analysis
To analyze the measured adhesion force induced by interlocking of line arrays,
Timoshenko beam theory is introduced to model the line structure as a thick
beam. It is generally acknowledged that Timoshenko beam theory is more
appropriate to explain the deformation of the beam than the simple beam
theory (also known as Euler-Bernoulli beam theory) when the thickness of the
beam is considerably larger than the length of the beam (i.e. low AR), since
the transverse shear deformation should be considered in that case.[29-31]
In
the case of implementing Timoshenko beam theory, the amount of the
deflection of the beam can be expressed as the combination of the deflection
predicted by the simple beam theory and additional term induced by
transverse shear force.[30]
With the boundary condition of clamped end at the
base and free end at the tip of the structure, deflection of the beam can be
denoted as
=
(
where denotes the deflection, 𝑀 is the bending moment, 𝑀 is the
bending moment at the base, G is the shear modulus (G =
2 1+𝜈 , 𝜈 is the
Poisson’s ratio), A is cross-sectional area, 𝜅 is the shear correction
coefficient (𝜅 = + 𝜈
+ 𝜈 for rectangular cross-section
[32]) and superscript T
and E indicates the corresponding term belongs to the Timoshenko beam
theory and Euler-Bernoulli beam theory.[30]
13
When the external load is induced by shear loading and the uniform load
distribution across the contact area is assumed, the deflection at the tip 𝛿𝑚𝑎𝑥
can be expressed as
𝛿𝑚𝑎𝑥 = 2 𝐿 (
𝐿2
𝐸𝐼
( )
2
𝜅 )
where is the applied shear force per single structure and is the overlap
ratio ( =𝑏
), respectively (Figure 6(a)). From experimental observations, the
average value of is estimated as 0.8. After all, the amount of the deflection
can be expressed as the function of the external shear force and overlap ratio.
14
3.2. Van der Waals force analysis and combined modeling
When the two line structures are brought into contact, van der Waals
interaction occurs at the contact surface and the van der Waals force per unit
area can be written as [33]
=
where denotes the Hamaker constant and is the cut-off distance
between surfaces which is assumed to be 0.4 nm.[33,34]
One thing to note is the
equation is based on the assumption that both two surfaces are nominally flat.
However, nanoscale roughness on the contact surface needs to be considered
because only a small amount of roughness can significantly affect the
variation of adhesion force.[34-37]
According to the previous researches, many
types of surface roughness can be modeled as a Gaussian distribution of
asperity heights.[38,39]
Also, contact between two rough surfaces can be
replaced as that of one nominally flat surface and one rough surface with
combined roughness.[40,41]
Then, the probability of area in contact between the
two identical surface, , can be derived as
=
2[ (
𝛿1 𝛿2 𝑚
2𝜎) (
𝑚
2𝜎)]
where erf denotes the error function, 𝛿1 = . 2𝜎1 2 𝜈2 𝐸 2
and 𝛿2 = 2. 2𝜎1 2 𝜈2 𝐸 2 is the minimum and maximum
amount of deformation predicted by Johnson-Kendall-Roberts (JKR) contact
15
model ( is the surface energy of s-PUA(=32.8 mJ/m2)
[42]), 𝜎 is the RMS
roughness of surface, 𝑚 is the maximum height of peak for the contacting
surface (approximated by 2.7 𝜎), (detailed derivation is shown in Ref.[40]
).
After substituting the measured value of 𝜎 (2.2 nm, Figure 6(b)), the value of
in the case of s-PUA is calculated to about 97 %, indicating that almost the
entire area is contacted with each other. However, this value falls into 15 %
when the contact of structure is made by h-PUA. It means the assumption of
the conformal contact is no longer valid, leading to lower adhesion force of h-
PUA surface as shown in Figure 4.
By applying revised van der Waals force which takes into account
nanoscale surface roughness and assuming the law of friction as (F = μN),
force equilibrium equation at a pair of interlocked line array is established
(Figure 6(a)). As shown, the interlocked line structure maintain the merged
state until
Where is the external shear force applied to the single structure, is
the van der Waals force at the contact surface, respectively. The paired
structure would begin to be separated when the inclined angle reaches critical
value ( 𝑐) that satisfies
𝑐 = 𝑐
from geometric approximation, 𝑐 𝛿𝑚𝑎𝑥 𝐿. By substituting 𝛿𝑚𝑎𝑥 to the
above force equilibrium equation, can be calculated. Then, the
macroscopic adhesion force can be estimated by multiplying the number of
paired structures per unit area. Since some portion of the array cannot be
16
interlocked due to uneven substrate, misalignment, and contaminants (e.g.
dust particles) (Figure 6(c)), the adhesion force of the whole system is
influenced by the locking ratio. In Figure 6(d), both Euler-Bernoulli and
Timoshenko beam bending theory predicts a monotonic increase in adhesion
force related with the locking ratio. Experimental results of adhesion force
with changing the locking ratio showed large discrepancy to the theoretical
value based on Euler-Bernoulli beam bending theory, while well matched to
the Timoshenko beam bending theory. This result shows the importance of
adopting the large deformation theory when considering the deflection of
relatively low AR structures.
17
4. Conclusion
18
A reversible interlocking system using regularly arrayed line array structure
has been presented. It can be fabricated by the simple UV-assisted molding
method. Designing rules for providing high adhesion force has been
investigated in terms of geometrical aspect and material characteristics. By
utilizing its structural robustness, long-term operation with repeatable
attachment and detachment was achieved without any notable degradation in
adhesion force. Also, a theoretical analysis using Timoshenko beam bending
theory and van der Waals force with nanoscale roughness has been conducted
to explain measured adhesion force. With further optimization based on the
analysis shown here, it might be possible to further enhance the performance
of the current line interlocking system.
19
Experimental section
20
Adhesion test
The adhesion test was conducted by the custom-built equipment (Figure 7). In
the measurement machine, the normal and shear adhesion force is measured
by load cell attached to each direction. The pre-aligned sample was loaded at
the flat stage and a preload of ~ 10 N/cm2 was applied. The adhesion force
was measured at least 10 times for each case and the averaged value was used.
Also, the measured adhesion value was divided by actual contact area to
calculate adhesion force per unit area (N/cm2). During the measurements, the
temperature of the stage was maintained at 20 ℃ and the relative humidity of
ambient was about 50%.
Field-Emission Scanning Electron Microscopy (FE-SEM)
SEM images were obtained by Auriga (Carl Zeiss, Germany) and S-4800
(Hitachi, Japan). To avoid charging effects, samples were coated with a Pt
film about ~ 5 nm thickness prior to measurements.
Atomic Force Microscopy (AFM)
AFM images were taken by a XE-150 (Park Systems, Korea) in noncontact
mode. The scan rate was 0.6 Hz and scan resolution was 256 x 256 pixels.
21
Figures
22
Figure 1. (a) Fabrication process of a PUA line array by two-step molding
method. (b) Schematic illustration of the interlocking procedure. (c) Cross-
sectional SEM image of fully interlocked line array.
23
Figure 2. (a) SEM images of the nanoscale line array (width=800 nm) with
three different spacing ratios (1, 3, and 5). The inset shows bird-view of the
each array. (b) Measured normal and shear adhesion force of samples.
24
Figure 3. (a) SEM images of the line structure array with three different
feature sizes (400 nm, 800 nm, and 5 μm). The inset shows bird-view of the
each array. (b) Plots showing a growing tendency of the adhesion force as
pattern size increases. (c-d) Macroscopic locking status and corresponding
cross-sectional SEM images of (c) 800 nm feature size and (d) 5um feature
size.
25
Figure 4. Adhesion graph showing normal and shear adhesion forces with
different materials.
26
Figure 5. (a) Measurement of adhesion forces with repeating cycles of
attachment and detachment up to ~250 cycles of normal direction and ~100
cycles of shear direction. (b) SEM images of a pristine line array sample and
the same after normal and shear repeatability test. (c) Two representative
failure modes of the protruded structure with different types of external loads.
27
Figure 6. (a) Schematic illustration of the deflection and force equilibrium of
the interlocked structure. (b) 3-D AFM image showing the nanoscale
roughness on the surface of the pattern. (c) Optical microscope images of the
interlocked line array, showing that locked and unlocked region is coexisted.
(d) Plots of expected shear adhesion force predicted by two types of beam
bending theories and measured adhesion force that follows Timoshenko beam
bending theory.
28
Figure 7. Photographs of a custom-built equipment used to measure the
normal and shear adhesion force of samples. A load cell is installed for each
direction and the pulling force is applied by motorized moving part.
29
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30
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33
요 약
본 논문은 자연계에 존재하는 다양한 생명체에서 찾아볼 수 있는
미세구조 기반의 가역적 상호체결 시스템에 대한 연구로, 자외선
경화성 고분자를 이용하여 제작된 선형 구조물 배열간의 상호체결
현상에 대한 연구를 수행하였다. 기존의 고종횡비 기둥 구조물 기반
상호체결 시스템의 문제점인 취약한 구조적 안정성으로 인한 낮은
반복성을 개선하는 것에 목표를 두었으며, 선형 구조물의 도입과
관련하여 체결 현상이 효과적으로 발생하기 위한 구조물 사이의
간격비와 패턴의 크기에 대한 기하학적 분석 및 재료의 탄성
계수에 의한 접착 성능의 차이를 관측하였다. 이를 통해 얻어진
최적화된 구조물의 형상을 기반으로 그 구조적 우수성을 확인하기
위한 반복성 실험 및 분석이 진행되었다. 체결된 구조물에서
발생하는 접착력의 크기는 접촉면에서의 힘의 평형을 통해 설명할
수 있는데, 종횡비가 낮은 선형 구조물의 변형을 고려하기 위해
단순 보 이론 대신 티모센코 (Timoshenko)보 이론을
도입하였으며, 또한 접촉면에 존재하는 나노스케일의 표면거칠기에
의한 영향을 고려하였다. 이와 같은 분석을 바탕으로 본 논문에서는
기존의 방법보다 더 정확하게 선형 구조물의 체결 현상 및 접착력
실험 결과를 설명할 수 있는 이론을 수립하였다.
주요어 : 자연모사, 가역적 상호체결시스템, 선형 구조물,
건식 접착, 반데르발스 힘
학 번 : 2012-22563