In this work, we report a large-area fabrication of a flexible superhydrophobic bactericidal surface decorated with copper hydroxide nanowires. This involves a simple two-step method which involves growth followed by transfer of the nanowires onto the polydimethylsiloxane (PDMS) surface by mechanical peeling. Additional roughness in PDMS is obtained through incomplete wetting of the nanoscale gaps which leads to dual-scale roughness and superhydrophobicity with a contact angle of 169° and hysteresis of less than 2°. The simplicity of the process makes it low-cost and easily scalable. The process allows fabrication of nonplanar 3D surfaces. The surface shows blood repellence and antibacterial activity against Escherichia coli with more than 5 log reductions in bacterial colony. The surface also shows hemocompatible behavior, making it suitable for healthcare applications. The fabricated surface is found to be extremely robust against stretching, twisting, sandpaper abrasion, solid weight impact, and tape peel test. The surface is found to withstand human weight multiple times without losing its hydrophobicity, making it suitable for several practical scenarios in healthcare and household applications.
Insects and plants exhibit bactericidal behavior through nanostructures, which leads to physical contact killing that does not require antibiotics or chemicals. Also, certain metallic ions (e.g., Ag and Cu) are well-known to kill bacteria by disrupting their cellular functionalities. The aim of this study is to explore the improvement in bactericidal activity by combining extreme physical structure with surface chemistry. We have fabricated tall (8-9 μm high) nanostructures on silicon surfaces (NSS) having sharp tips (35-110 nm) using a single-step, maskless deep reactive ion etching technique inspired by dragonfly wing. Bactericidal efficacy of the nanostructured surfaces coated with a thin layer of silver (NSS_Ag) or copper (NSS_Cu) was measured quantitatively using standard viability plate-count method and flow cytometry. NSS_Cu surfaces kill bacteria very efficiently (killing 97% within 30 min) when compared to the uncoated NSS. This can be attributed to the addition of a surface chemistry to the nanostructures. The antibacterial activity of NSS_Cu is further indicated by the morphological differences of the dying/dead bacteria observed in the SEM images. The nanostructured surfaces demonstrate excellent superhydrophobic behavior, even with an ultrathin layer of metal (Ag/Cu) coating. The nanostructured surfaces exhibit static contact angle greater than 150° and contact hysteresis less than 10°. Moreover, reflectance is found to be <1% (for NSS_Cu < 0.5%) for all the nanostructured surfaces in the wavelength range 250-800 nm. The results obtained suggest that the fabricated nanostructured surfaces are multifunctional and can be used in various practical applications.
Functional ZnO nanostructured surfaces are important in a wide range of applications. Here we report the simple fabrication of ZnO surface structures at near room temperature with morphology resembling that of sea urchins, with densely packed, µm-long, tapered nanoneedles radiating from the urchin center. The ZnO urchin structures were successfully formed on several different substrates with high surface density and coverage, including silicon (Si), glass, polydimethylsiloxane (PDMS), and copper (Cu) sheets, as well as Si seeded with ZnO nanocrystals. Time-resolved SEM revealed growth kinetics of the ZnO nanostructures on Si, capturing the emergence of "infant" urchins at the early growth stage and subsequent progressive increases in the urchin nanoneedle length and density, whilst the spiky nanoneedle morphology was retained throughout the growth. ε-Zn(OH) 2 orthorhombic crystals were also observed alongside the urchins. The crystal structures of the nanostructures at different growth times were confirmed by synchrotron X-ray diffraction measurements. On seeded Si substrates, a two-stage growth mechanism was identified, with a primary growth step of vertically aligned ZnO nanoneedle arrays preceding the secondary growth of the urchins atop the nanoneedle array. The antibacterial, anti-reflective, and wetting functionality of the ZnO urchins-with spiky nanoneedles and at high surface density-on Si substrates was demonstrated. First, bacteria colonization was found to be suppressed on the surface after 24 h incubation in gram-negative Escherichia coli (E. coli) culture, in contrast to control substrates (bare Si and Si sputtered with a 20 nm ZnO thin film). Secondly, the ZnO urchin surface, exhibiting superhydrophilic property with a water contact angle ∼ 0 • , could be rendered superhydrophobic with a simple silanization step, characterized by an apparent water contact angle θ of 159 • ± 1.4 • and contact angle hysteresis ∆θ < 7 • . The dynamic superhydrophobicity of the surface was demonstrated by the bouncing-off of a falling 10 µL water droplet, with a contact time of 15.3 milliseconds (ms), captured using a high-speed camera. Thirdly, it was shown that the presence of dense spiky ZnO nanoneedles and urchins on the seeded Si substrate exhibited a reflectance R < 1% over the wavelength range λ = 200-800 nm. The ZnO urchins with a unique morphology fabricated via a simple route at room temperature, and readily implementable on different substrates, may be further exploited for multifunctional surfaces and product formulations.
Functional ZnO nanostructured surfaces are important in a wide range of applications. Here we report facile fabrication of ZnO surface structures at near room temperature with morphology resembling that of sea urchins, with densely packed, μm-long, tapered nanoneedles radiating from the urchin centre. The ZnO urchin structures were successfully formed on several different substrates with high surface density and coverage, including silicon (Si), glass, polydimethylsiloxane (PDMS), and copper (Cu) sheets, as well as Si seeded with ZnO nanocrystals. Time-resolved SEM revealed growth kinetics of the ZnO nanostructures on Si, capturing the emergence of “infant” urchins at the early growth stage and subsequent progressive increase in the urchin nanoneedle length and density, whilst the spiky nanoneedle morphology was retained throughout the growth. ε-Zn(OH)2 orthorhombic crystals were also observed alongside the urchins. The crystal structures of the nanostructures at different growth time were confirmed by synchrotron X-ray diffraction measurements. On seeded Si substrates, a two-stage growth mechanism was identified, with a primary growth step of vertically aligned ZnO nanoneedle arrays preceding the secondary growth of the urchins atop the nanoneedle array. The antibacterial, anti-reflective, and wetting functionality of the ZnO urchins—with spiky nanoneedles and at high surface density—on Si substrates was demonstrated. First, bacteria colonisation was found to be suppressed on the surface after 24 h incubation in Gram-negative E. coli culture, in contrast to control substrates (bare Si and Si sputtered with 20 nm ZnO thin film). Secondly, the ZnO urchin surface, exhibiting superhydrophilic property with a water contact angle ~0°, could be rendered superhydrophobic with a simple silanization step, characterised by a water static contact angle θ of 159° ± 1.4° and contact angle hysteresis ∆θ < 7°. The dynamic superhydrophobicity of the surface was demonstrated by bouncing-off of a falling 10 μL water droplet, with a contact time of 15.3 milliseconds (ms), captured using a high-speed camera. Thirdly, it was shown that the presence of dense spiky ZnO nanoneedles and urchins on the seeded Si substrate exhibited a reflectance R < 1% over the wavelength range λ = 200–800 nm. The ZnO urchins with unique morphology via a facile fabrication route at room temperature, readily implementable on different substrates, may be further exploited for multifunctional surfaces and product formulations.
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