Submicron Feature Sizes Research Articles

3D-patterned inverse-designed mid-infrared metaoptics

Modern imaging systems can be enhanced in efficiency, compactness, and application through the introduction of multilayer nanopatterned structures for manipulation of light based on its fundamental properties. High transmission multispectral imaging is elusive due to the commonplace use of filter arrays which discard most of the incident light. Further, given the challenges of miniaturizing optical systems, most cameras do not leverage the wealth of information in polarization and spatial degrees of freedom. Optical metamaterials can respond to these electromagnetic properties but have been explored primarily in single-layer geometries, limiting their performance and multifunctional capacity. Here we use advanced two-photon lithography to realize multilayer scattering structures that achieve highly nontrivial optical transformations intended to process light just before it reaches a focal plane array. Computationally optimized multispectral and polarimetric sorting devices are fabricated with submicron feature sizes and experimentally validated in the mid-infrared. A final structure shown in simulation redirects light based on its angular momentum. These devices demonstrate that with precise 3-dimensional nanopatterning, one can directly modify the scattering properties of a sensor array to create advanced imaging systems.

Scalable Fabrication of Nanogratings on GaP for Efficient Diffraction of Near-Infrared Pulses and Enhanced Terahertz Generation by Optical Rectification

We present a process flow for wafer-scale fabrication of a surface phase grating with sub-micron feature sizes from a single semiconductor material. We demonstrate this technique using a 110-oriented GaP semiconductor wafer with second-order nonlinearity to obtain a nanostructured device (800 nm lateral feature size and a 245 nm height modulation) with applications relevant to near-infrared optical diffraction and time-resolved terahertz (THz) technologies. The fabrication process involves a plasma-enhanced chemical deposition of a SiO2 layer on the wafer followed by contact photolithography and inductively coupled plasma reactive ion etching (ICP-RIE). We discuss the required radiation dosage, exposure times, temperatures and other key parameters to achieve high-quality nanogratings in terms of filling ratio, edge profile, and overall shape. The phase-grating properties, such as the pitch, spatial homogeneity, and phase retardation, are characterized with an atomic force microscope, scanning electron microscope and a non-invasive optical evaluation of the optical diffraction efficiency into different orders. We demonstrate an application of this device in a time-domain THz spectroscopy scheme, where an enhanced THz spectral bandwidth is achieved by optical rectification of near-infrared laser pulses incident on the grating and efficiently diffracted into the first orders. Finally, the reported process flow has the potential to be applied to various materials by considering only slight adjustments to the ICP-RIE etching steps, paving the way to scalable fabrication of sub-micron patterns on a large range of substrates.

On the potential use of two-photon polymerization to 3D print chromatographic packed bed supports

The continuous quest for chromatographic supports offering kinetic performance properties superior to that of the packed bed of spheres has pushed the field to consider alternative formats such as for example monolithic and pillar array columns. This quest seems bound to culminate in the use of 3D printing technology, as this intrinsically offers the possibility to produce supports with a perfect uniformity and with a size and shape that is fully optimized for the chromatographic separation process. However, to be competitive with the current state-of-the-art, structures with sub-micron feature sizes are required. The present contribution therefore investigates the use of the 3D printing technology with the highest possible resolution available today, i.e., two-photon polymerization (2PP). It is shown that 2PP printing is capable of achieving the required ≤ 1 µm printing resolution. Depending on the laser scan speed, the lower limit through-pore size for a tetrahedral skeleton monolith with a theoretical 80% external porosity was found to be at 800 nm, when printing at a scan speed of 50 mm/s with a laser power of 10%. For a scan speed of 10 mm/s, the minimal through-pore size dropped to 500 nm. However, this very high resolution comes at the cost of excessively long printing times. The total printing time for a column volume equivalent to that of a typical nano-LC column (75 µm i.d. cylindrical tube with length L = 15 cm) has been determined to correspond to 330 and 470 h for the 50 mm/s and the 10 mm/s scan speed respectively. Other issues remaining to be solved are the need to clad the printed skeleton with a suitable mesoporous layer for chromatographic retention and the need to add a top-wall to the printed channels after the removal of the non-polymerized resin. It is therefore concluded that 2PP printing is not ready yet to replace the existing column fabrication methods.

Nanoscale focused electron beam induced etching of nickel using a liquid reactant

Nickel nanostructures have found widespread application as both functional components, e.g. in magnetic systems, and as part of the lithographic pattern transfer process as etch masks, EUV mask absorbers, and imprint templates. Electron-beam induced etching of nickel is highly desirable for the repair and editing of masks and templates with high resolution and without substrate damage. However, there are no known gas-phase reactants that produce volatile nickel products under e-beam irradiation. Here we report the successful local etching of nickel by a focused electron beam in an environmental scanning electron microscope using a liquid reactant, aqueous sulfuric acid. Sulfuric acid did not spontaneously etch nickel under ESEM conditions, but nickel was etched in areas exposed to the electron beam. Etching parameters such as dose, refresh time, and addition of a surfactant were investigated. The extent of the etch increases with dose before terminating at sub-micron feature sizes. The etch resolution improves with the addition of surfactant. This approach enables local nickel patterning with complete film removal but without damaging underlying layers. With further refinement, the process may enable nickel absorber repair and editing and remove a significant obstacle to the use of nickel in EUV lithography.

Thermodynamic-driven polychromatic quantum dot patterning for light-emitting diodes beyond eye-limiting resolution

The next-generation wearable near-eye displays inevitably require extremely high pixel density due to significant decrease in the viewing distance. For such denser and smaller pixel arrays, the emissive material must exhibit wider colour gamut so that each of the vast pixels maintains the colour accuracy. Electroluminescent quantum dot light-emitting diodes are promising candidates for such application owing to their highly saturated colour gamuts and other excellent optoelectronic properties. However, previously reported quantum dot patterning technologies have limitations in demonstrating full-colour pixel arrays with sub-micron feature size, high fidelity, and high post-patterning device performance. Here, we show thermodynamic-driven immersion transfer-printing, which enables patterning and printing of quantum dot arrays in omni-resolution scale; quantum dot arrays from single-particle resolution to the entire film can be fabricated on diverse surfaces. Red-green-blue quantum dot arrays with unprecedented resolutions up to 368 pixels per degree is demonstrated.

Large-size updatable optically addressed spatial light modulator (OASLM) based on ZnO nanoparticles for large-area holographic 3D displays

Optically addressed spatial light modulators (OASLMs) provide an appropriate solution for large-area and wide-viewing angle holographic displays because of the possibility of uploading holograms on it through tiling and with sub-micron diffraction feature sizes. A prototype with a large-size OASLM of 100 mm × 100 mm was fabricated using a solution-based deposition process for ZnO nanoparticles (NPs). ZnO NP-based OASLM is suitable for hologram tiling because of the extended charge carrier lifetime as a result of trap states in the ZnO NP layer annealed at a low temperature of 180°C, of which the activation energy was determined firstly by low-temperature measurements. Operating the ZnO NP OASLM in a DC driving mode was subsequently proposed, to utilize the extended charge carrier lifetime in the photosensor layer for temporary information storage. Finally, techniques to tile computer generated holograms (CGHs) spatially on a single OASLM were explored and evaluated, including the demonstration of simultaneous image replay from sequentially tiled two separate phase-only CGHs.

Polycarbonate Heat Molding for Soft Lithography.

Soft lithography enables rapid microfabrication of many types of microsystems by replica molding elastomers into master molds. However, master molds can be very costly, hard to fabricate, vulnerable to damage, and have limited casting life. Here, an approach for the multiplication of master molds into monolithic thermoplastic sheets for further soft lithographic fabrication is introduced. The technique is tested with master molds fabricated through photolithography, mechanical micromilling as well as 3D printing, and the results are demonstrated. Microstructures with submicron feature sizes and high aspect ratios are successfully copied. The copying fidelity of the technique is quantitatively characterized and the microfluidic devices fabricated through this technique are functionally tested. This approach is also used to combine different master molds with up to 19 unique geometries into a single monolithic copy mold in a single step displaying the effectiveness of the copying technique over a large footprint area to scale up the microfabrication. This microfabrication technique can be performed outside the cleanroom without using any sophisticated equipment, suggesting a simple way for high-throughput rigid monolithic mold fabrication that can be used in analytical chemistry studies, biomedical research, and microelectromechanical systems.

Scalably manufactured textured surfaces for controlling wettability in oil-water systems

Competitive wettability in oil-water systems influences applications such as oil-water separation and enhanced oil recovery. Here, we study the wettability of water (in oil) and oil (in water) on sub-millimeter/micro/nano textured surfaces fabricated on a variety of substrates (metals, polymers, elastomers). Importantly, all the fabrication processes employed involved non-cleanroom-based scalable techniques. Metal surfaces were fabricated via wet etching processes and polymer/elastomer surfaces were fabricated via laser etching. These fabrication techniques can enable texturing with sub-millimeter, micron and sub-micron feature sizes. Wettability was characterized by measuring static contact angle and dynamic contact angle (roll-off angle). Several insights into wettability are obtained from this work. Firstly, textured metal surfaces with low energy surface chemistry showed the lowest adhesion to water and oil droplets. Textured metal surfaces coated with Teflon AF were superhydrophobic (in oil) with very low roll-off angles (4°–7°). Uncoated textured metal surfaces were superoleophobic (in water) with roll-off angles of 3°–9°. Secondly, textured polymer and elastomer surfaces exhibited utrahydrophobicity (in oil); however not all textured elastomers exhibited superoleophobicity (in water). Thirdly, no droplet roll-off was observed on any textured elastomer and polymer surface, despite very favourable contact angles. This indicates that high contact angles do not always translate to superhydrophobicity/oleophobicity. Fourthly, it is seen that competitive wettability of a surface can be understood by analysing the corresponding water and oil wettability of that surface in an air environment. Additionally, the initial state of the surface can be important, as the first fluid in contact with the surface fills the porous textures, and dictates subsequent wettability. All these findings and insights position this work as the foundation for more detailed studies on the development of surfaces for specific applications.

Printing sub-micron structures using Talbot mask-aligner lithography with a 193 nm CW laser light source.

A continuous improvement of resolution in mask-aligner lithography is sought after to meet the requirements of an ever decreasing minimum feature size in back-end processes. For periodic structures, utilizing the Talbot effect for lithography has emerged as a viable path. Here, by combining the Talbot effect with a continuous wave laser source emitting at 193 nm, we demonstrate successfully the fabrication of periodic arrays in silicon substrates with sub-micron feature sizes. The excellent coherence and the superior brilliance of this light source, compared to more traditional mercury lamps and excimer lasers as light source, enables the efficient beam shaping and a reduced minimum feature size at a fixed gap of 20 µm. We present a comprehensive study of proximity printing with this system, including simulations and selected experimental results of prints in up to the fourth Talbot plane. This printing technology can be used to manufacture optical metasurfaces, bio-sensor arrays, membranes, or microchannel plates.

Adaptive stitching for meso-scale printing with two-photon lithography

An inevitable trade-off between resolution and total size exists when 3D printing objects. This is also the case for two-photon or multi-photon lithography. While it is capable of reaching a sub-micron feature size, it needs to combine a high precision movement mechanism with a lower precision one when writing centimetric size objects. As a result, the final part consists of a combination of many individual blocks, where the overlapping areas often create bumps and imperfections in the final object. In the current contribution, we demonstrate how an adaptive stitching algorithm can lead to a reduction in the total amount of stitching blocks of up to 40% for slender objects (i.e. with features smaller than the individual block size). As is demonstrated on a winding microfluidic channel, this can lead to substantial manufacturing time gains of up to 25%. As our tiling is irregular, we also explain how to create the writing masks for the blocks and decide on their order. In the special case in which one does not need to print one single large continuous part, but rather many individual ones (such as a microlens array), we demonstrate how zero-overlap stitching can be achieved with a modified version of our adaptive algorithm.

Energy‐efficient fault tolerant technique for deflection routers in two‐dimensional mesh Network‐on‐Chips

New generation multi-processor system-on-chips integrate hundreds of processing elements in a single chip which communicate with each other through on-chip communication networks, commonly known as network-on-chip (NoC). Routers are the most critical NoC components and deflection routing is a technique used in buffer-less routers for better energy efficiency. Massive integration of devices along with fabrication at deep sub-micron level feature sizes increases the possibility of wear out and damage to various components resulting in unreliable operation of the chip. Hence NoC fabric in general and routers, in particular, should be equipped with built-in fault tolerance mechanisms to ensure the reliability of the chip in the presence of faults. The authors propose an energy-efficient routing technique that can tolerate permanent faults in NoC links by introducing a simple logic unit placed next to the output port allocation stage of the deflection router pipeline. This technique incurs minimum wiring overheads and promises a stable network throughput for high fault rates. Evaluation of the proposed method on 8 × 8 mesh NoC for various fault rates reports reduced flit deflection rate and hop power which brings about a significant reduction in dynamic power consumption at the inter-router links compared to state-of-the-art fault tolerance techniques.

Optical anisotropy in vertically oriented TiO2 nanotube arrays

Nanofabricated optically anisotropic uniaxial thin films with deep submicron feature sizes are emerging as potential platforms for low-loss all-dielectric metamaterials, and for Dyakonov surface wave-based subwavelength optical confinement and guiding at interfaces with isotropic media. In this context, we investigate the optical properties of one such uniaxial platform, namely self-organized titania nanotube arrays (TNTAs) grown by the bottom-up nanofabrication process of electrochemical anodization on silicon wafer substrates, and subsequently annealed at different temperatures, i.e. 500 °C and 750 °C. We performed detailed quantitative analysis of the structure of the TNTAs using x-ray diffraction and Raman spectroscopy, which revealed a measurable phonon confinement in TNTAs annealed at 500 °C. Variable angle spectroscopic ellipsometry was used to investigate the optical anisotropy in two kinds of TNTAs—those constituted by anatase-phase and those containing a mixture of anatase and rutile phases. Both kinds of TNTAs were found to have positive birefringence (Δn) exceeding 0.06 in the spectral region of interest while mixed phase TNTAs exhibited Δn as high as 0.15. The experimentally measured anisotropy in the refractive index of the TNTAs was compared with the predictions of two different effective medium approximations incorporating the uniaxial geometry. The measured value of Δn for TNTAs exceeded that of bulk anatase single crystals, indicating the potential of nanostructured dielectrics to outperform dielectric crystals of the same material with respect to the magnitude of the achievable directional refractive index contrast.

Fluorescent sensing with Fresnel microlenses for optofluidic systems

The concept of fluorescent sensing in a microchannel equipped with focusing light Fresnel lenses has been demonstrated. The concept employs a line or array of Fresnel lenses generating a line or array of focused light spots within a microfluidic channel, to increase the sensitivity of fluorescent signal detection in the system. We have presented efficient methods of master mold fabrication based on the lithography method and focused ion beam milling. The flexible microchannel was fabricated by an imprint process with new thiolene-epoxy resin with a good ability to replicate even submicron-size features. For final imprinted lenses, the measured background to peak signal level shows more than nine times the increase in brightness at the center of the focal spot for the green part of the spectrum (532 nm). The effectiveness of the microlenses in fluorescent-marked Escherichia coli bacteria was confirmed in a basic fluoroscope experiment, showing the increase of the sensitivity of the detection by the order of magnitude.

Effect of electrode sub-micron surface feature size on current generation of Shewanella oneidensis in microbial fuel cells

Abstract Microbial fuel cells (MFCs) are envisioned to serve as compact and sustainable sources of energy; however, low current and power density have hindered their widespread use. Introduction of 3D micro/nanostructures on the MFC anode is known to improve its performance by increasing the surface area available for bacteria attachment; however, the role of the feature size remains poorly understood. To delineate the role of feature size from the ensuing surface area increase, nanostructures with feature heights of 115 nm and 300 nm, both at a height to width aspect ratio of 0.3, are fabricated in a grid pattern on glassy carbon electrodes (GCEs). Areal current densities and bacteria attachment densities of the patterned and unpatterned GCEs are compared using Shewanella oneidensis Δ bfe in a three-electrode bioreactor. The 115 nm features elicit a remarkable 40% increase in current density and a 78% increase in bacterial attachment density, whereas the GCE with 300 nm pattern does not exhibit significant change in current density or bacterial attachment density. The current density dependency on feature size is maintained over the entire 160 h experiment. Thus, optimally sized surface features have a substantial effect on current production that is independent of their effect on surface area.

Scanning SQUID susceptometers with sub-micron spatial resolution.

Superconducting QUantum Interference Device (SQUID) microscopy has excellent magnetic field sensitivity, but suffers from modest spatial resolution when compared with other scanning probes. This spatial resolution is determined by both the size of the field sensitive area and the spacing between this area and the sample surface. In this paper we describe scanning SQUID susceptometers that achieve sub-micron spatial resolution while retaining a white noise floor flux sensitivity of ≈2μΦ0/Hz1/2. This high spatial resolution is accomplished by deep sub-micron feature sizes, well shielded pickup loops fabricated using a planarized process, and a deep etch step that minimizes the spacing between the sample surface and the SQUID pickup loop. We describe the design, modeling, fabrication, and testing of these sensors. Although sub-micron spatial resolution has been achieved previously in scanning SQUID sensors, our sensors not only achieve high spatial resolution but also have integrated modulation coils for flux feedback, integrated field coils for susceptibility measurements, and batch processing. They are therefore a generally applicable tool for imaging sample magnetization, currents, and susceptibilities with higher spatial resolution than previous susceptometers.

Fabrication of submicron proteinaceous structures by direct laser writing

In this paper, we provide a characterization of truly free-standing proteinaceous structures with submicron feature sizes depending on the fabrication conditions by model-based analysis. Protein cross-linking of bovine serum albumin is performed by direct laser writing and two-photon excitation of flavin adenine dinucleotide. We analyze the obtainable fabrication resolution and required threshold energy for polymerization. The applied polymerization model allows prediction of fabrication conditions and resulting fabrication size, alleviating the application of proteinaceous structure fabrication.

Phase shifting masks in Displacement Talbot Lithography for printing nano-grids and periodic motifs

High-resolution periodic structures with geometric shapes such as squares or triangles cannot be readily produced with low-cost photolithography methods like interference or proximity photolithography. We present a method for robust printing of such patterns with Displacement Talbot Lithography (DTL) using phase shifting masks. This combination effectively yields high-contrast images that extend to large distances from the mask. It therefore enables uniform images to be printed over large, non-flat substrates without loss of resolution. Phase masks with several different motifs have been designed, fabricated and tested using DTL exposures. High-fidelity grid and island type structures with square and triangular motifs and sub-micron feature sizes were printed into different types of photoresists using wafer–mask gaps on the order of 100μm. The experimental results show good agreement with calculated image intensity distributions. The method is suitable for low-cost production of high-quality patterned growth substrates and photonic structures among other applications.

Electrets in soft materials: nonlinearity, size effects, and giant electromechanical coupling.

Development of soft electromechanical materials is critical for several tantalizing applications such as soft robots and stretchable electronics, among others. Soft nonpiezoelectric materials can be coaxed to behave like piezoelectrics by merely embedding charges and dipoles in their interior and assuring some elastic heterogeneity. Such so-called electret materials have been experimentally shown to exhibit very large electromechanical coupling. In this work, we derive rigorous nonlinear expressions that relate effective electromechanical coupling to the creation of electret materials. In contrast to the existing models, we are able to both qualitatively and quantitatively capture the known experimental results on the nonlinear response of electret materials. Furthermore, we show that the presence of another form of electromechanical coupling, flexoelectricity, leads to size effects that dramatically alter the electromechanical response at submicron feature sizes. One of our key conclusions is that nonlinear deformation (prevalent in soft materials) significantly enhances the flexoelectric response and hence the aforementioned size effects.

Rapid fabrication of micron‐sized CVD‐diamond structures by microfluidic contact printing

In this contribution we report on a novel method for the growth of laterally patterned synthetic diamond films with submicron feature sizes. The lateral patterning is induced by depositing a nanodiamond‐based seeding layer prior to the chemical vapor deposition of the diamond films. The seeding layer is prepared by a microfluidic approach, based on soft lithography with PDMS moulds, used in the microcontact printing. These moulds are prepared by electron‐beam lithography of photoresist on silicon substrates. The master moulds are reusable, allowing for cheap, high‐throughput manufacturing, and the resulting diamond microstructures exhibit an outstanding smoothness and structural reproducibility. Possible applications are expected in the fields of diamond electronics, micro‐electro‐mechanical systems (MEMS) as well as bio‐ and chemosensors. The abstract figure shows the SU‐8 master mould (left). The resulting diamond structure (right) is shown, after chemical vapor deposition. The purple color originates from the settings of the optical microscope, used to get a high‐contrast image.

Direct Laser Writing Facility for Fabrication of Submicron Mask

Direct laser writing technique has become a well-established, multi-functional and flexible method for fabricating high quality diffractive optical elements. We propose and build a maskless direct laser writing system with the ability to produce a sub-micron feature size. The high precision lithography is realized by using the astigmatic autofocus method. The minimum feature size of the system, breaking through the diffraction limit with the chromium layer, can achieve 300 nm with the 405 nm blue laser. A 50 × 50 mm2 chromium grating mask with a period of 1 μm and line width of 300 nm is fabricated. This facility will be useful for the fabrication of large-scale submicron diffraction optical elements in the future.