# 1 Gecko-Inspired Nanomaterials

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5 1.2 The Physics of Gecko Adhesion 5 (a) P s Interfacial contact area (b) P s Smooth interfacial contact W s 2a s W s Smooth peel adhesive P s = 2(G c w s ) P s = 8πG c E * a s 3 Smooth adhesive P n Patterned contact area P n Pattern post interface 2a f W f W f Patterned peel adhesive P n = n ½ P s P n = n ¼ P s Figure 1.3 Examples demonstrating the principle of contact splitting. For both examples, the separation force of the patterned adhesive ( P n ) increases with the total number of split - up contacts ( n ), which illustrates that the enhancement in strength is associated with the increase in contact line, as opposed to contact area. (a) In a peel Patterned adhesive geometry, P n n 1/2 ; (b) In a flat-punch geometry, P n n 1/4. G c is the interfacial adhesion, a s is the smooth contact radius, E * is the reduced Young s modulus, and P s is the separation force for a smooth reference. Figure reproduced from Ref. [9] ; 2007, Materials Research Society. separation would actually decrease because of a reduction in the interfacial contact area. In order for patterns to increase both total force and total energy, the energy associated with initiating separation at the perimeter of an individual post must be greater than the energy of propagation away from the perimeter. This may be caused by differences in mechanical constraints, and has been demonstrated to cause significant increases in adhesion for some patterned interfaces [15, 18 20]. A second example of how patterns may change the interfacial contribution can be explained by considering the perpendicular separation of a pillar from a flat surface (e.g., a finger pulling away from a sticky surface) (Figure 1.3 b). In this case, it can easily be shown that the force to separate n posts ( P n ) scales directly with the separation force of a single post ( P s ) [21] : P n = n 1/4 P s. The scaling changes if the posts are terminated with spherical caps of a curvature R. In this situation, Johnson Kendall Roberts (JKR ) theory [22] predicts that P n = n 1/2 P s [7], such that the interfacial strength is enhanced by reducing the diameter of the pillars [23]. Similar to the peeling examples above, the energy of separation is enhanced only if the initiation energy is greater than the propagation energy. Although the example mechanisms discussed here consider energy dissipation only at the interface, the three - dimensional (3 - D) geometry of a patterned interface also has an important role to play. In this case, the aspect ratio of the features

8 8 1 Gecko-Inspired Nanomaterials Figure 1.5 Adhesion design map for a flat tip against a substrate with periodical roughness. For the surface roughness, a radius of the small spheres of a = 500 nm is considered. The dashed, orange line is the conode. For R > 500 nm, the presented model for flat tips against a rough surface is employed. For R > a, the apparent contact strength is constant over the entire map contact splitting invariance and the minimum Young s modulus is determined by the fi ber fracture limit. Reproduced with permission from Ref. [26]. to that of the gecko fibrillar system, at ca. 55 ). An example of a design map that takes into account surface roughness is shown in Figure 1.5. Whilst this might be only a first step, it clearly shows that adhesion design maps represent a versatile tool for visualizing the design parameters that are important for fibrillar adhesives, and might also prove very useful in the future development of such systems. Finally, it must be stressed that, despite the many simplifications made (some of which were quite severe) when constructing the maps, these predictions have proven to be intriguingly accurate. 1.3 Fabrication Methods for Gecko -Inspired Adhesives Soft-Molding Among the most common methods used to fabricate fibrillar adhesives, the best - known is that of soft lithography [27]. The term itself is applied to a collection of pattern - replication methods which rely on an elastomeric mold [27, 28]. The latter

9 1.3 Fabrication Methods for Gecko-Inspired Adhesives Figure 1.6 SEM image of a PDMS test surface structured via soft lithography. The pillars are 10 μm in radius and have an aspect ratio of 1. The image demonstrates the high quality and homogeneity of soft-lithographic structures. is a negative replica of a microstructured or nanostructured hard master, and is prepared by casting and thermally curing a liquid prepolymer (most often poly(dimethylsiloxane); PDMS) on the master. The PDMS replica can be considered as the ﬁnal patterned surface (Figure 1.6), or it can also be used as a mold (or stamp) for patterning other polymeric materials in subsequent replication processes. The elastomeric character of the PDMS stamp allows it to be released easily from the master (or molded polymer), even in the presence of complex and fragile structures, such as high-aspect ratio ﬁbers. Moreover, its low interfacial free energy and chemically inertness reduce the degree of mold sticking. One prerequisite for soft-molding is access to masters with a desired geometry. The masters for bioinspired ﬁbrillar adhesives consist of arrays of holes with predeﬁned dimensions, and have been typically fabricated by photolithography [15, 16, 29, 30]. Alternatively, masters have been produced by indenting a wax surface with an AFM tip [31], or by the laser ablation of a metallic surface [32]. Photolithography using an SU-8 photoresist has been proven particularly suited to obtaining regular model surfaces in which the inﬂuence of the different geometric parameters on adhesion can be characterized and quantiﬁed [16]. This resist material has been specially formulated to obtain high-aspect ratio features, such as holes, which are required to obtain long PDMS ﬁbers in the replication process [33]. Arrays of ﬁbers with radii of 1 to 25 μm and lengths of 5 to 80 μm have been reported over 25 cm2 areas [16]. These systems have been used to analyze the inﬂuence of contact radius and aspect ratio of the ﬁbers in the ﬁnal adhesion performance of the artiﬁcial adhesive surface [16]. In theory, soft-molding allows the fabrication of ﬁbers of any dimensions, but in reality the aspect ratio of the ﬁbers is limited by the low mechanical stability of the PDMS, with ﬁber collapse 9

10 10 1 Gecko-Inspired Nanomaterials Figure 1.7 SEM image showing an array of pillars made by soft - molding Sylgard 184 onto SU - 8 photolithographic templates. The pillars have a radius of 2.5 μ m and a height of about 20 μ m. The image highlights the collapse of pillars with hexagonal symmetry. Reprinted with permission from Ref. [16]. typically occurring in micron -sized fibers with aspect ratios in excess of 4 (Figure 1.7 ). This fact is more critical in nanosized fibers, the fabrication of which requires the use of harder materials. Soft PDMS stamps can be also applied to generate fibrillar micropatterns of different materials by soft - molding polymer melts, polymer solutions, or polymer precursors. For example, PDMS stamps have been used to soft - mold liquid polyurethane precursors, such that fibers with 20 μ m diameter, 40 to 100 μm length and 40 μ m spacings were obtained [34]. In addition, PDMS is transparent and can be used to mold UV - curable prepolymers; in this case, hard polyurethane patterns with fibrils of 0.5 to 4 μ m height and diameters ranging from 1 to 4 μ m have been created [30]. Tilted fibrillar structures are required if reversible gecko - inspired adhesives are to be fabricated. The tilted disposition of the fibers allows the adhesive to be peeled - off, and therefore easily removed [35]. Tilted SU - 8 fibrils have been obtained via photolithography by tilting the mask and the resist film with respect to the beam during exposure, using a tilting stage. In this way, soft - molding polyurethane precursors with a PDMS negative replica of the SU - 8 master yielded arrays of polyurethane microfibers with a tilting angle of 25 [34]. By using a polyurethane instead of PDMS, the group of Metin Sitti from Carnegie Mellon University also created several fibrillar adhesives with tilted pillars [34, 36]. In another very interesting approach, Pokroy et al. [37] fabricated nanoposts with different tilt angles via a two - step soft - molding process where, in the second step, the PDMS mold was stretched, compressed, and torsioned in various ways.

11 1.3 Fabrication Methods for Gecko-Inspired Adhesives Nanostructured Adhesive Surfaces Hot Embossing Thermoplastic materials can be patterned by the process of hot embossing, in which a polymer melt is shaped by the conformal contact of a microstructured or nanostructured mold, using heat and pressure. The polymer melt is able to flow and fill the mold cavities under the processing conditions. The filling depends on the viscosity of the melt, its wetting properties and pattern geometry, as well as on applied pressure or vacuum. Solidification of the polymer after filling is achieved by cooling below the crystallization temperature in semicrystalline polymers, or below the glass transition temperature ( T g ) in amorphous polymers. Removal of the mold releases a structured polymer with features that reproduce its particular geometry; this is achieved by either peeling - off (demolding) or by a selective dissolution of the template. Demolding is preferred as it permits the same mold to be used for additional molding processes. The embossing process was carried out at temperatures above the T g of poly(methylmethacrylate) (PMMA ) ( 120 C), using a polyurethane acrylate mold, such that arrays of fibers of 150 nm diameter and up to 500 nm in height were obtained [38, 39]. The fabrication of high - quality molds represents one of the most important requirements for successful embossing. These molds are typically prepared from silicon or silicon dioxide by dry - etching technologies, or by the deposition of nickel or other metals on patterned resist substrates, via the LIGA ( Lithographie, Galvanofomung, and Abformungprocess ) process. Since mold fabrication is the most time - and cost - consuming step of these patterning techniques, it is likely to constitute the greatest limitation in potential industrial applications Filling Nanoporous Membranes Track-etched polycarbonate (PC ) and anodic alumina (AA ) membranes have been used as low - cost alternatives to expensive molds for producing arrays of long, nanosized fibers [31, 40, 41]. These membranes are commercially available, with pore sizes ranging from a few nanometers to a few micrometers, and with different spacings and thicknesses. The pores of the membrane can be filled with polymer precursors, solutions or melts so as to obtain a structured polymer film possessing cylinders with dimensions that reproduce those of the pores (Figure 1.8 ). This method has been used quite extensively for the first examples of fibrillar adhesives [31, 40, 41]. PC membranes containing randomly distributed cylindrical pores of 0.6 μm diameter and spacings <5 μ m have been filled with poly(imide) (PI ) solutions [40]. As the PC membrane is flexible, it can be peeled - off from the solidified PI film to release dense arrays of high - aspect ratio nanofibers. Due to their large aspect ratio, these fibers were shown to collapse laterally, and therefore a reduced adhesion would be expected. AA membranes with pores of nm diameter have been also filled with a two - parts epoxy resin [40], with a polystyrene ( PS )

12 12 1 Gecko-Inspired Nanomaterials Figure 1.8 Cross-sectional view of as-prepared and vertically aligned polystyrene nanotubes fabricated through the fi lling of a porous membrane. Note the bundling of the fi bers. Reproduced with permission from Ref. [41] ; Wiley-VCH Verlag GmbH & Co. KGaA. solution [41], and with UV - curable precursors [42]. Because of their rigidity, AA membranes cannot be removed from the polymer by peeling - off, but rather need to be dissolved selectively in NaOH solution. Unfortunately, this represents a major disadvantage for fabrication, as the template is destroyed, while dissolution takes a long time and may also cause polymer swelling. Wet etching is also followed by a drying step, during which capillary forces usually may cause lateral collapse and, consequently, reduced adhesion (Figure 1.8 ) [42]. Similar problems of fiber condensation were also reported by Kim et al. [43], who used colloidal nanolithography to fabricate the mold for their parylene nanopillars Electron-Beam Lithography Arrays of PI fibers have been microfabricated using electron - beam lithography ( EBL ), followed by pattern transfer via dry etching in an oxygen plasma [44]. The etching step is necessary in order to obtain high - aspect ratio structures, as the maximum penetration depth of low - energy electrons is only about 100 nm. The diameters of the fibers produced ranged from 0.2 to 4 μ m, the heights from 0.15 to 2 μ m, and the spacings from 0.4 to 4.5 μ m. Whilst this method is appropriate for obtaining model nanostructures with smaller dimensions than are obtained via optical photolithography, the patterning is slow, is restricted to small areas, and also requires an electron - beam facility to be available.

13 1.3 Fabrication Methods for Gecko-Inspired Adhesives Carbon Nanotubes Microfabrication techniques strongly restrict the material s selection to some resists, all of which are quite expensive. In addition, patterning can only be carried out in specialized laboratories (clean rooms), and requires costly equipment and long processing times. For this reason, the quest has begun for alternative patterning techniques that do not require a template (e.g., the mold in soft - lithography or the mask in photolithography). Consequently, arrays of vertically aligned carbon nanotube s ( CNT s) have been reported as an interesting alternative [45 50]. CNTs have smaller diameters (10 20 nm) than gecko spatulae ( 200 nm), and may also be made with high length ( >65 μ m [46] ). In having an extremely high aspect ratio, exceptional mechanical strength, and excellent electronic and thermal properties, CNTs show great potential for dry adhesion applications with additional electrical/thermal management capabilities (e.g., electroswitching, through - thickness thermal transport, high - temperature use) [45]. Arrays of CNTs have also been fabricated via chemical vapor deposition ( CVD ) on Si substrates, where the nanotubes were aligned almost perpendicular to the substrate surface and had a fairly uniform tubular length. Unfortunately, however, they tended to stick to their closest neighbors, forming loosely-packed bundles that reduced the overall adhesive force of the CNT layer due to a lesser number of contact points. Arrays of CNTs were successfully transferred from the Si wafer to flexible backing substrates [46, 47]. For this purpose, the patterned silicon wafer was embedded in a polymer precursor and, after curing, the CNTs were peeled - off from the wafer. By etching the silicon - facing side of the polymer matrix, either by solvents or through plasma treatment, a smooth layer of CNTs was generated on a flexible backing Drawing Polymer Fibers Arrays of nanofibers have been obtained by drawing fibers from polymer drops on nonwettable surfaces by contacting them with a hot plate and then moving the two surfaces apart [51]. This process is based on surface tension and capillary forces, and is available in several versions. For example, films of thermoplastic polymers can be brought in contact with a hot structured master possessing pillars; subsequently, when the master and the polymer are pulled apart, fibers will be drawn from the contacting points. Alternatively, structured polymer films with large features can be brought in contact with a hot surface and then removed, so as to obtain elongated fibers on the top of the features [51]. Others have developed a miniaturized version of this method by using an AFM tip to draw nanosized fibers from a melt polymer film [52]. Although these fabrication methods seemed more suited to large - area patterning, and were therefore more likely to be applied in manufacturing systems, the production of nanosized fibers would require a concise alignment between the hot plate (or roll) and the polymer film, across large areas. An ingenious alternative was reported recently which avoided alignment problems by combining the molding and fiber drawing processes so as to obtain high-aspect ratio nanofibers from thin PS and PMMA films [53]. This was achieved by carrying out the demolding step at temperatures above the T g -values

15 1.3 Fabrication Methods for Gecko-Inspired Adhesives (1) Coating photoresist, soft bake (4) 2nd masked irradiation SU-8 Si water (2) Masked irradiation (5) Development Mask (3) Coating new photoresist layer (6) Soft molding, demolding 100 μm Figure 1.9 Schematic of the processing steps for the fabrication of hierarchical PDMS pillars through two-step photolithography and soft-molding. The lower panel shows an SEM image showing an array of hierarchical pillars fabricated by soft-molding Sylgard 184 on SU-8 photolithographic templates. The base-pillars have a radius of 25 μm and a height of 200 μm. The top pillars have a radius of 5 μm and an aspect ratio of 1. The right-hand insert shows a close-up of the hierarchical structure; the left-hand inset shows a water droplet resting on the structure (contact angle 160 ). The arrows indicate pillar sections. Reproduced with permission from Ref. [54]; Wiley-VCH Verlag GmbH & Co. KGaA Two-Step Embossing By performing two sequential embossing steps, hierarchical patterns with micrometric ﬁbers decorated with nanosized ﬁbers of various sizes and spacings were obtained [38]. A PMMA ﬁlm was patterned with microﬁbers using a PDMS stamp; subsequently, nanoﬁbers were patterned on top of the preformed microﬁbers, using a hard polyurethane acrylate (PUA) mold. The 15

16 16 1 Gecko-Inspired Nanomaterials PUA mold replaces the PDMS mold for sub nm lithography, since high - aspect ratio sub nm features in a PDMS mold do not retain dimensional stability, due to the low Young s modulus of PDMS. The resultant micro/nanoscale combined structures were robust, and demonstrated enhanced water - repellent properties as a consequence of the hierarchical arrangement D Structured Adhesive Surfaces The 3 - D geometry of the tip seems to be crucial for the adhesion performance of a fibrillar surface, with spherical, conical, filament-like, band-like, sucker-like, spatula-like, flat and toroidal tip shapes having been observed in different animals [60]. The role of the contact geometry has also been analyzed in artificial model systems [17], with a study conducted by del Campo et al. revealing that the contact shape had a strong influence on adhesion [17]. Using a modification of the soft - molding method, arrays of PDMS fibers with spherical and spatula - like tips have been reported [17, 61, 62]. The fabrication methods employed are shown in Figure Here, arrays of pillars with spherical and spatular tips were obtained by inking PDMS fibrillar surfaces in a thin film of the PDMS precursor. A small drop of precursor remained on the top of the pillars. Curing of the array in an upside - down orientation yielded hemispherical tips as a consequence of gravity and surface tension acting on the fluid drop. Alternatively, the inked stamp could be pressed against a flat substrate and then cured, so as to create pillars with a flexible 1) Soft molding (complete filling of master cavities) and curing 1) Spin coat a thin film and wait for partial hardening (delay time, t d ) 2) Demolding Elastomeric array of pillars Elastomer precursor SU-8 master 3) Inking Thin film of elastomer precursor 4) Downwards curing 4) Printing, curing 4) Tilted printing, curing Film of elastomer precursor 2) Retarded molding (partial filling) t d1 >> SU-8 master t d2 Planar contacts Spherical tips Symmetric spatulae θ Asymmetric spatulae Tubes Coucave tips 20 μm 20 μm 20 μm 20 μm 20 μm 20 μm (a) (b) (c) (d) (e) (f) Figure 1.10 Overview of the fabrication strategies for PDMS pillars with different tip shapes, as developed by del Campo et al. The SEM images (a f) show examples of the structures obtained. Reproduced with permission from Ref. [61]; Wiley-VCH Verlag GmbH & Co. KGaA.

18 18 1 Gecko-Inspired Nanomaterials Figure 1.11 SEM images of Tecoﬂex pillars with r = 10 μm, h = 100 μm and 20 μm interpillar spacing. (a) Original pattern; (b) Top (left) and side (right) views of tilted pillars after deformation at 70 C and ﬁxation in the deformed state by cooling below Ttrans; (c) Top (left) and side (right) views of recovered pillars after reheating at 70 C. Reproduced with permission from Ref. [65]; Wiley-VCH Verlag GmbH & Co. KGaA. applied driving force is greater than a critical value (Gc), then the two materials will separate. When Gc is known for a given pair of materials, the practical design parameters such as the maximum sustainable force or stress for a given geometry can be determined. Frequently, contact probe adhesion tests are used for both patterned and nonpatterned interfaces. In contact probe testing, a probe is brought into contact with another material, and the established interface is subsequently separated [18, 69, 70]. During the entire test, the force (P), the displacement (δ), and the contact area (A = πa2, where a is the radius) are monitored and provide a complete description of the adhesion

31 1.6 Applications in the Life Sciences Figure 1.18 Development of biodegradable synthetic gecko patterns. (a) Nanomolding of the GSA prepolymer is accomplished by photocuring the prepolymer under UV light, followed by removal of the pattern and subsequent spin coating of DXTA on the surface of the pillars. SEM imaging demonstrated excellent pattern transfer and ﬁdelity; (b) Gecko patterns having different pillar size and center-to-center pitch were developed, as illustrated in the SEM images. Pillar dimensions were measured by using optical proﬁlometry, as represented by the bar graphs, with red representing the height of pillars; black the center-to-center pitch; light gray the diameter of pillar base; and dark gray the diameter of the tip. Small and large scale bars are 1 and 10 μm, respectively; (c) Adhesion trend of the longest pillar heights (2.4 μm) shows adhesion of the nanopattern with respect to ﬂat polymer as a function of ratio of tip diameter to pitch. The R2 value of linear ﬁt was 0.99; (d) Adhesion trend of the patterns plotted as a function of the ratio of tip diameter to base diameter of pillars. The R2 values of linear ﬁts for the low- and high-pitch patterns were 0.96 and 0.99, respectively. Reprinted from Ref. [111]; 2008, National Academy of Sciences, USA. 31

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