Abstract:Titanium (Ti) represents a promising new material for microelectromechanical systems (MEMS) because of its unique properties. Recently, this has been made possible with the advent of processes that enable deep reactive ion etching (DRIE) of high-aspect-ratio (HAR) structures in bulk Ti substrates. However, to date, these processes have been limited to minimum feature sizes (MFS) ≥750 nm. Although this is sufficient for many applications, MFS reduction to the deep submicrometer range opens potential for further… Show more
“…The thinner ridge walls also suggest that as more reactive species became available, the tendency for isotropic etching increased, which led to increased etching of the wall surface. Similar trends have been reported by other researchers ,, and were also observed with nanopillars in this study. While at 30 sccm flow, thick and free-standing pillars were obtained, as the flow rate was increased to 40 sccm, the pillars became relatively thinner.…”
Section: Resultssupporting
confidence: 93%
“…At 50 sccm, the pillars became wirelike, much thinner, and with a greater tendency to clump together, which likely results from increased mechanical instability (Figures a and S2b). This reduction in diameter is similar to the increased sidewall etching in the patterned etching of titanium …”
Section: Resultssupporting
confidence: 52%
“…This reduction in diameter is similar to the increased sidewall etching in the patterned etching of titanium. 36 Therefore, taken together, the gas flow rate and chamber pressure decide the availability of reactive ions that interact with the substrate, their incoming energy (mean free path), and the duration of their stay in the chamber (residence time) (Figures 2c and 3c). Inside a clean chamber, this leads to similar trends on the morphology and etch rate of nanostructures for both these parameters, whereas opposite trends are observed inside an unclean chamber due to a higher concentration of masking species.…”
Bioinspired nanostructured antibacterial surfaces are among the most promising recent discoveries in nanotechnology to tackle microbial colonization of surfaces, especially with the growing challenge of antimicrobial resistance. Reactive ion etching (RIE) is one of the few nanofabrication techniques that has been demonstrated to be capable of generating biomimetic nanostructures on large substrates through a combination of physical and chemical etching. However, the physics behind the formation of these structures and their spatiotemporal evolution is poorly understood, primarily limited by the challenges associated with placing in situ characterization instruments inside the process chamber. The limited understanding in the field leads to poor reproducibility, constraining the widespread acceptance and application of this technique. This work describes maskless RIE of commercially pure titanium substrates using chlorine and fluorine plasma. It is demonstrated that the chamber condition plays a critical role toward determining the morphology of the nanostructures generated, and high aspect ratio (HAR) nanostructures can be generated reproducibly by following proper cleaning protocols involving fluorine plasma by scavenging the SiOCl species that accumulate in the chamber walls over time. Furthermore, the control of several process parameters to reproducibly fabricate various types of nanostructures such as nanoridges, nanopillars, and nanowires are demonstrated, along with insights into the underlying physical principles. HAR nanopillars are generated, and their bactericidal mechanism and efficiency are shown to be primarily dependent on their aspect ratio. This study provides insights to resolve the hitherto poorly understood events of fabrication of bioinspired nanostructures by RIE with important implications for reliably and reproducibly engineering biomaterial surfaces with bactericidal activity.
“…The thinner ridge walls also suggest that as more reactive species became available, the tendency for isotropic etching increased, which led to increased etching of the wall surface. Similar trends have been reported by other researchers ,, and were also observed with nanopillars in this study. While at 30 sccm flow, thick and free-standing pillars were obtained, as the flow rate was increased to 40 sccm, the pillars became relatively thinner.…”
Section: Resultssupporting
confidence: 93%
“…At 50 sccm, the pillars became wirelike, much thinner, and with a greater tendency to clump together, which likely results from increased mechanical instability (Figures a and S2b). This reduction in diameter is similar to the increased sidewall etching in the patterned etching of titanium …”
Section: Resultssupporting
confidence: 52%
“…This reduction in diameter is similar to the increased sidewall etching in the patterned etching of titanium. 36 Therefore, taken together, the gas flow rate and chamber pressure decide the availability of reactive ions that interact with the substrate, their incoming energy (mean free path), and the duration of their stay in the chamber (residence time) (Figures 2c and 3c). Inside a clean chamber, this leads to similar trends on the morphology and etch rate of nanostructures for both these parameters, whereas opposite trends are observed inside an unclean chamber due to a higher concentration of masking species.…”
Bioinspired nanostructured antibacterial surfaces are among the most promising recent discoveries in nanotechnology to tackle microbial colonization of surfaces, especially with the growing challenge of antimicrobial resistance. Reactive ion etching (RIE) is one of the few nanofabrication techniques that has been demonstrated to be capable of generating biomimetic nanostructures on large substrates through a combination of physical and chemical etching. However, the physics behind the formation of these structures and their spatiotemporal evolution is poorly understood, primarily limited by the challenges associated with placing in situ characterization instruments inside the process chamber. The limited understanding in the field leads to poor reproducibility, constraining the widespread acceptance and application of this technique. This work describes maskless RIE of commercially pure titanium substrates using chlorine and fluorine plasma. It is demonstrated that the chamber condition plays a critical role toward determining the morphology of the nanostructures generated, and high aspect ratio (HAR) nanostructures can be generated reproducibly by following proper cleaning protocols involving fluorine plasma by scavenging the SiOCl species that accumulate in the chamber walls over time. Furthermore, the control of several process parameters to reproducibly fabricate various types of nanostructures such as nanoridges, nanopillars, and nanowires are demonstrated, along with insights into the underlying physical principles. HAR nanopillars are generated, and their bactericidal mechanism and efficiency are shown to be primarily dependent on their aspect ratio. This study provides insights to resolve the hitherto poorly understood events of fabrication of bioinspired nanostructures by RIE with important implications for reliably and reproducibly engineering biomaterial surfaces with bactericidal activity.
“…the most common areas of applications for such profiles) 50 . Furthermore, the resulting nanostructures of the Cl 2 gas have vertical sidewalls and smoother surfaces 51 . We therefore chose Cl 2 /Ar chemistry and studied the effects of gas flows on the Ti structures.…”
One of the major problems with the bone implant surfaces after surgery is the competition of host and bacterial cells to adhere to the implant surfaces. To keep the implants safe against implant-associated infections, the implant surface may be decorated with bactericidal nanostructures. Therefore, fabrication of nanostructures on biomaterials is of growing interest. Here, we systematically studied the effects of different processing parameters of inductively coupled plasma reactive ion etching (ICP RIE) on the Ti nanostructures. The resultant Ti surfaces were characterized by using scanning electron microscopy and contact angle measurements. The specimens etched using different chamber pressures were chosen for measurement of the mechanical properties using nanoindentation. The etched surfaces revealed various morphologies, from flat porous structures to relatively rough surfaces consisting of nanopillars with diameters between 26.4 ± 7.0 nm and 76.0 ± 24.4 nm and lengths between 0.5 ± 0.1 μm and 5.2 ± 0.3 μm. The wettability of the surfaces widely varied in the entire range of hydrophilicity. The structures obtained at higher chamber pressure showed enhanced mechanical properties. The bactericidal behavior of selected surfaces was assessed against Staphylococcus aureus and Escherichia coli bacteria while their cytocompatibility was evaluated with murine preosteoblasts. The findings indicated the potential of such ICP RIE Ti structures to incorporate both bactericidal and osteogenic activity, and pointed out that optimization of the process conditions is essential to maximize these biofunctionalities.
“…Most wet etching methods produce isotropic shapes on the target materials. However, when we used potassium hydroxide (KOH), ethylenediamine pyrocatechol, tetramethylammonium hydroxide, or metal-assisted chemical etching, anisotropic shapes could be formed. − For anisotropic etching, a dry etching process is usually preferred. − It avoids the use of hazardous and toxic solutions that may be required in wet etching. Dry etching can also be used to change the surface properties such as the hydrophilicity and surface profile (shape and roughness) by controlling the pressure, type of etching gas, and voltage and power of the bias in the plasma electrode. − However, undercutting, profile tilting, notching, bowing effects, loading effects, and charging effects during the surface treatment or surface etching must be overcome to produce a purposed nanostructure while maintaining their anisotropic shape and purposed surface profile. − …”
Recently,
researchers have dedicated efforts toward producing large-area
nanostructures using advanced lithography techniques and state-of-the-art
etching methods. However, these processes involve challenges such
as the diffraction limit and an unintended etching profile. In this
work, we demonstrate large-area nanopatterning on a silicon substrate
using the microscale metal mask by meticulous optimization of the
etching process. Around the vertex of a microscale metal mask, a locally
induced electric field is generated by a bias voltage applied on a
silicon mold. We utilize this field to change the trajectory of reactive
ions and their effect flux, thus providing a controllable bowing effect.
The results are analyzed by both numerical simulations and experiments.
Based on the field alignment by the metal mask for the etching (FAME)
process, we demonstrate the fabrication of 378 nm-size nanostructure
patterns which translate to a size reduction of 63% from 1 μm-size
mask patterns on a wafer by optimization of the processes. This is
much higher than the undercut (∼37%) usually achieved by a
typical non-Bosch process under similar etching conditions. The optimized
nanostructure is used as a mold for the transfer printing of nanostructure
arrays on a flexible substrate to demonstrate that it enables the
functionality of FAME-processed nanostructures.
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