Magnetization dynamics in single and trilayer nanowires.

We have studied the magnetization dynamics of single Py(t) (t= 20 nm, 50 nm) and trilayer [Py(50)/Pd(tPd)/Py(20)] nanowire arrays fabricated over large areas using deep ultraviolet lithography technique. The dynamic properties are sensitive to the field orientation and magnetic film thicknesses. A single resonant mode corresponding to the excitations at the bulk part of the wire is detected in all the single-layer nanowire arrays. Furthermore, the spacer layer thickness influenced the dynamic properties in trilayer samples due to the different coupling mechanisms. A single resonant mode is observed intPd= 2 nm trilayer nanowires with a sharp frequency jump from 13 GHz to 15 GHz across the reversal regime. This indicates the exchange coupling and the coherence in magnetization precession in the ferromagnetic layers. On the other hand, wires with 10 nm-spacer display two well-resolved modes separated by ∼3 GHz with a gradual change in frequency across the reversal regime from-26mT to-46mT, indicating the presence of long-range dipolar interactions instead of exchange coupling. The spacer layer of the proposed spin-valve-type structure can be tailored for desired microwave splitters or combiners.

Facile Fabrication of Hierarchical Structured Anodic Aluminum Oxide Molds for Large-Scale Production of Superhydrophobic Polymer Films.

Anodized aluminum oxide (AAO) molds were used for the production of large-area and inexpensive superhydrophobic polymer films. A controlled anodization methodology was developed for the fabrication of hierarchical micro-nanoporous (HMN) AAO imprint molds (HMN-AAO), where phosphoric acid was used as both an electrolyte and a widening agent. Heat generated upon repetitive high-voltage (195 V) anodization steps is effectively dissipated by establishing a cooling channel. On the HMN-AAO, within the hemispherical micropores, arrays of hexagonal nanopores are formed. The diameter and depth of the micro- and nanopores are 18/8 and 0.3/1.25 µm, respectively. The gradual removal of micropatterns during etching in both the vertical and horizontal directions is crucial for fabricating HMN-AAO with a high aspect ratio. HMN-AAO rendered polycarbonate (PC) and polymethyl methacrylate (PMMA) films with respective water contact angles (WCAs) of 153° and 151°, respectively. The increase in the WCA is 80% for PC (85°) and 89% for PMMA (80°). On the PC and PMMA films, mechanically robust arrays of nanopillars are observed within the hemispherical micropillars. The micro-nanopillars on these polymer films are mechanically robust and durable. Regular nanoporous AAO molds resulted in only a hydrophobic polymer film (WCA = 113-118°). Collectively, the phosphoric acid-based controlled anodization strategy can be effectively utilized for the manufacturing of HMN-AAO molds and roll-to-roll production of durable superhydrophobic surfaces.

Direct deep UV lithography to micropattern PMMA for stem cell culture.

Microengineering is increasingly being used for controlling the microenvironment of stem cells. Here, a novel method for fabricating structures with subcellular dimensions in commonly available thermoplastic poly(methyl methacrylate) (PMMA) is shown. Microstructures are produced in PMMA substrates using Deep Ultraviolet lithography, and the effect of different developers is described. Microgrooves fabricated in PMMA are used for the neuronal differentiation of mouse embryonic stem cells (mESCs) directly on the polymer. The fabrication of 3D, curvilinear patterned surfaces is also highlighted. A 3D multilayered microfluidic chip is fabricated using this method, which includes a porous polycarbonate (PC) membrane as cell culture substrate. Besides directly manufacturing PMMA-based microfluidic devices, an application of the novel approach is shown where a reusable PMMA master is created for replicating microstructures with polydimethylsiloxane (PDMS). As an application example, microchannels fabricated in PDMS are used to selectively expose mESCs to soluble factors in a localized manner. The described microfabrication process offers a remarkably simple method to fabricate for example multifunctional topographical or microfluidic culture substrates outside cleanrooms, thereby using inexpensive and widely accessible equipment. The versatility of the underlying process could find various applications also in optical systems and surface modification of biomedical implants.

Microfabrication Process Development for a Polymer-Based Lab-on-Chip Concept Applied in Attenuated Total Reflection Fourier Transform Infrared Spectroelectrochemistry.

Micro electro-mechanical systems (MEMS) combining sensing and microfluidics functionalities, as are common in Lab-on-Chip (LoC) devices, are increasingly based on polymers. Benefits of polymers include tunable material properties, the possibility of surface functionalization, compatibility with many micro and nano patterning techniques, and optical transparency. Often, additional materials, such as metals, ceramics, or silicon, are needed for functional or auxiliary purposes, e.g., as electrodes. Hybrid patterning and integration of material composites require an increasing range of fabrication approaches, which must often be newly developed or at least adapted and optimized. Here, a microfabrication process concept is developed that allows one to implement attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) and electrochemistry on an LoC device. It is designed to spatially resolve chemical sensitivity and selectivity, which are instrumental for the detection of chemical distributions, e.g., during on-flow chemical and biological reaction chemistry. The processing sequence involves (i) direct-write and soft-contact UV lithography in SUEX dry resist and replication in polydimethylsiloxane (PDMS) elastomers as the fluidic structure; (ii) surface functionalization of PDMS with oxygen plasma, 3-aminopropyl-triethoxysilane (APTES), and a UV-curable glue (NOA 73) for bonding the fluidic structure to the substrate; (iii) double-sided patterning of silicon nitride-coated silicon wafers serving as the ATR-FTIR-active internal reflection element (IRE) on one side and the electrode-covered substrate for microfluidics on the back side with lift-off and sputter-based patterning of gold electrodes; and (iv) a custom-designed active vacuum positioning and alignment setup. Fluidic channels of 100 µm height and 600 µm width in 5 mm thick PDMS were fabricated on 2" and 4" demonstrators. Electrochemistry on-chip functionality was demonstrated by cyclic voltammetry (CV) of redox reactions involving iron cyanides in different oxidation states. Further, ATR-FTIR measurements of laminar co-flows of H2O and D2O demonstrated the chemical mapping capabilities of the modular fabrication concept of the LoC devices.

Bionic Tactile-Gustatory Receptor for Object Identification Based on All-Polymer Electrochemical Transistor.

Human sensory receptors enable the real world to be perceived effortlessly. Hence, massive efforts have been devoted to the development of bionic receptors capable of identifying objects. Unfortunately, most of the existing devices are limited to single sensory emulation and are established on solid-state electronic technologies, which are incompatible with the biological reactions occurring in electrolyte media. Here, an iontronic tactile-gustatory receptor using an all-polymer electrochemical transistor (AECT) is presented. The sensor is biocompatible with the operation voltage of 0.1 V, which is 1 to 2 orders lower than those of reported values. By this study, one receptor is able to accurately recognize various objects perceived by the human tactile and gustatory system without complex circuitry. Additionally, to promote its further application, flexible AECT arrays with channel length of 2 µm and density of 104 167 transistors cm-2 (yield of 97%) are fabricated, 1 to 5 orders higher than those of related works. Finally, a flexible integrated network for electrocardiogram recording is successfully constructed. This study moves a step forward toward state-of-the-art bionic sensors.

Experimental Validation of Diffraction Lithography for Fabrication of Solid Microneedles.

Microneedles are highly sought after for medicinal and cosmetic applications. However, the current manufacturing process for microneedles remains complicated, hindering its applicability to a broader variety of applications. As diffraction lithography has been recently reported as a simple method for fabricating solid microneedles, this paper presents the experimental validation of the use of ultraviolet light diffraction to control the liquid-to-solid transition of photosensitive resin to define the microneedle shape. The shapes of the resultant microneedles were investigated utilizing the primary experimental parameters including the photopattern size, ultraviolet light intensity, and the exposure time. Our fabrication results indicated that the fabricated microneedles became taller and larger in general when the experimental parameters were increased. Additionally, our investigation revealed four unique crosslinked resin morphologies during the first growth of the microneedle: microlens, first harmonic, first bell-tip, and second harmonic shapes. Additionally, by tilting the light exposure direction, a novel inclined microneedle array was fabricated for the first time. The fabricated microneedles were characterized with skin insertion and force-displacement tests. This experimental study enables the shapes and mechanical properties of the microneedles to be predicted in advance for mass production and wide practical use for biomedical or cosmetic applications.

Polystyrene Pocket Lithography: Sculpting Plastic with Light.

Tissue-culture-ware polystyrene is the gold standard for in vitro cell culture. While microengineering techniques can create advanced cell microenvironments in polystyrene, they require specialized equipment and reagents, which hinder their accessibility for most biological researchers. An economical and easily accessible method is developed and validated for fabricating microstructures directly in polystyrene with sizes approaching subcellular dimensions while requiring minimal processing time. The process involves deep ultraviolet irradiation through a shadow mask or ink pattern using inexpensive, handheld devices followed by selective chemical development with common reagents to generate micropatterns with depths/heights between 5 and 10 µm, which can be used to guide cell behavior. The remarkable straightforwardness of the process enables this class of microengineering techniques to be broadly accessible to diverse research communities.

Three-Dimensional Micropatterning Deters Early Bacterial Adherence and Can Eliminate Colonization.

Developing strategies to prevent bacterial infections that do not rely on the use of drugs is regarded globally as an important means to stem the tide of antimicrobial resistance, as argued by the World Health Organization (WHO) (Mendelson, M.; Matsoso, M. P. The World Health Organization Global Action Plan for Antimicrobial Resistance. S. Afr. Med. J. 2015, 105 (5), 325-325. DOI: 10.7196/SAMJ.9644). Given that many antimicrobial-resistant infections are caused by the bacterial colonization of indwelling medical devices such as catheters and ventilators, the use of microengineered surfaces to prevent the initial attachment of microbes to these devices is a promising solution. In this work, it is demonstrated that 3D engineered surfaces can inhibit the initial phases of surface colonization for Escherichia coli, Klebsiella pneumoniae, and Pseudomonas aeruginosa, representing the three most common catheter-associated urinary tract bacterial infections, identified by the WHO as urgent threats. A variety of designs including 11 different topographies and configurations that exhibited random distributions, sharp protrusions, and/or curvilinear shapes with dimensions ranging between 500 nm and 2 µm were tested to better understand the initial stages of surface colonization and how to optimize the design of fabricated surfaces for improved inhibition. These topographies were fabricated in two configurations to obtain either a standard 2D cross section or a 3D engineered topography using a novel UV lithography process enabling cost-efficient high-throughput manufacturing. Evaluating both the number of adhered bacteria and microcolonies formed by all three bacterial pathogens on the different surfaces provides insight into the initial colonization phase of bacterial growth on the various surfaces. The results demonstrate that both initial attachment and subsequent colonization can be significantly reduced on concrete 3D engineered patterns when compared to flat substrates and standard 2D micropatterns. Thus, this technology has great potential to reduce the colonization of bacteria on surfaces in clinical settings without the need for chemical treatments that might enhance antimicrobial resistance.

Enhancing the soft-tissue integration of dental implant abutments-in vitro study to reveal an optimized microgroove surface design to maximize spreading and alignment of human gingival fibroblasts.

Within this work, we demonstrate the influences of different microgrooved surface topographies on the alignment and spreading of human gingival fibroblast (HGF) cells and present the optimal parameters for an improved soft-tissue integration design for dental implant abutments for the first time. Microgrooves with lateral widths from 2.5 to 75 µm were fabricated by UV-lithography and wet etching on bulk Ti6Al4V ELI material. The microstructured surfaces were compared to polished and ground surfaces as current state of the art. The resulting microtopographies were analyzed using vertical scanning interferometry and scanning electron microscopy. Samples loaded with HGF cells were incubated for 8 and 72 hr and cell orientation, spreading, resulting area, and relative gene expression were analyzed. The effect of contact guidance occurred on all microstructured surfaces yet there is a clear preferable range for the lateral widths of the microgrooves between approx. 11.5 and 13.9 µm and depths between 1.6 and 2.4 µm for an abutment surface design, where cell orientation and spreading maximizes. For structures larger than 30 µm, cell orientation, spreading and even gene expression of intercellular adhesion molecule-1 and yes-associated protein decrease.

Lithographic Performance of Aryl Epoxy Thermoset Resins as Negative Tone Photoresist for Microlithography.

Photoresists (or photo-resins) are the main and most important raw material used for lithography techniques such as deep X-ray (DXRL), ultraviolet (UVL), deep-UV (DUVL), and extreme UV (EUVL). In previous work, we showed how complicated could be the synthesis of the resins used to produce photoresist. In this study, we follow up on the strategy of tuning deep and macro levels of properties to formulate photo-resins. They were developed from a primary basis, using epoxy resins, a solvent, and a photoinitiator in several concentrations. The formulations were evaluated initially by the UVL technique, using a squared pattern of 2.3 mm2. The most suitable compositions were then studied in a pattern structure varying from 50 down to 1 µm width, applying UVL and DUVL. The patterned structures were compared with the chemical composition of the photo-resins. Considering the deep level of properties, polydispersion, and epoxidation degree were evaluated. Regarding the macro level of properties, the concentration of photoinitiator was studied. Promising results have been achieved with the control of the deep and macro levels methodology. By means of UV lithography, it was possible to note, for a large feature size above 2.0 mm2, the formulations presented good quality structures with a broad range of epoxidation degrees and photoinitiator concentrations, respectively from 3 to 100% (mol·molpolymer-1) and from 10 to 40% (mol·molpolymer-1). For structures smaller than 50 µm width, the composition of the photo-resins may be restricted to a narrow range of values regarding the formulation. The results indicate that the polydispersion of the oligomers might be a significant property to control. There is a tendency to better outcome with a low polydispersity (resins P1 and P2). Regarding UV and deep-UV irradiation, the best results were achieved with UV. Nevertheless, for DUV, the sensitivity seems to be more intense, leading to well-defined structures with over-exposure effects.

Synthesis Based on a Preceramic Polymer and Alumina Nanoparticles via UV Lithography for High Temperature Applications.

Because of the increased demand for preceramic polymers in high-tech applications, there has been growing interest in the synthesis of preceramic polymers, including polysiloxanes and alumina. These polymers are preferred because of their low thermal expansion, conformability to surfaces over large areas, and flexibility. The primary objective was to evaluate the aspects of polymer-derived ceramic routs, focusing on the UV lithography process of preceramic polymers and the pyrolyzing properties of the final ceramics. We found that the p(DMS-co-AMS) copolymer was effective in scattering the hydrophilic Al2O3 nanoparticles into the exceedingly hydrophobic solvent. The physico-chemical behavior of characterized copolymers was explored during their pyrolytic transformation into amorphous silicon-based ceramics. The results indicate that an increase of the pyrolysis temperature degraded the Si-O network through the carbothermic reaction of silicon. We also found a rapid elimination of copolymer pores and densification when the temperature increased (1100 to 1200 °C). At different but specific temperature ranges, there are different distinct rearrangement reactions in the conversion of polymer to ceramic; reductions of the melting point (Tm) of the total heat of melting (ΔHm) of the pyrolysis process resulted in the crystallization of ceramic materials; hence, lithography based on pyrolysis properties of preceramic polymers is a critical method in the conversation of polymers.

3D Microlithography Using an Integrated System of 5-mm UV-LEDs with a Tilt-Rotational Sample Holder.

This paper demonstrates a 3D microlithography system where an array of 5 mm Ultra Violet-Light Emitting Diode (UV-LED) acts as a light source. The unit of the light source is a UV-LED, which comes with a length of about 8.9 mm and a diameter of 5 mm. The whole light source comprises 20 × 20 matrix of such 5 mm UV-LEDs giving a total number of 400 LEDs which makes it a very favorable source with a large area for having a batch production of the desired microstructures. This light source is able to give a level of precision in microfabrication which cannot be obtained using commercial 3D printers. The whole light source performs continuous rotational movement once it is turned on. This can also move up and down in a vertical direction. This multidirectional light source also comprises a multidirectional sample holder. The light source teaming up with the multidirectional sample holder highly facilitates the process of fabrication of a huge range of 3D structures. This article also describes the different levels of characterization of the system and demonstrates several fabricated 3D microstructures including high aspect ratio vertical micro towers, twisted turbine structures, triangles, inclined pillar 'V' structures, and hollow horn structures as well.

Plasmonic Lithography Utilizing Epsilon Near Zero Hyperbolic Metamaterial.

In this work, a special hyperbolic metamaterial (HMM) metamaterial is investigated for plasmonic lithography of period reduction patterns. It is a type II HMM (ϵ∥ < 0 and ϵ⊥ > 0) whose tangential component of the permittivity ϵ∥ is close to zero. Due to the high anisotropy of the type II epsilon-near-zero (ENZ) HMM, only one plasmonic mode can propagate horizontally with low loss in a waveguide system with ENZ HMM as its core. This work takes the advantage of a type II ENZ HMM composed of aluminum/aluminum oxide films and the associated unusual mode to expose a photoresist layer in a specially designed lithography system. Periodic patterns with a half pitch of 58.3 nm were achieved due to the interference of third-order diffracted light of the grating. The lines were 1/6 of the mask with a period of 700 nm and ∼1/7 of the wavelength of the incident light. Moreover, the theoretical analyses performed are widely applicable to structures made of different materials such as silver as well as systems working at deep ultraviolet wavelengths including 193, 248, and 365 nm.

A Novel Bioinspired Continuous Unidirectional Liquid Spreading Surface Structure from the Peristome Surface of Nepenthes alata.

A novel unidirectional liquid spreading surface with an inclined arc pitted groove, inspired by the continuous unidirectional liquid spreading mechanism on the peristome surface of N. alata, is explored and fabricated by two-step UV lithography. Its superior unidirectional liquid spreading capability to that of other surface patterns is demonstrated, and its unidirectional liquid spreading mechanism is investigated.

Hydrogel with Orthogonal Reactive Units: 2D and 3D Cross-Linking Modulation.

In this work, an engineered hydrogel system with a 2D and 3D tunable cross-linking degree is presented. A precise chemical design by the introduction of cross-linkable units, having reaction orthogonality, allows to control the network formation both in time and space and to selectively alter the hydrogel physical properties. Hydrogel chemistry has been tailored in order to produce spatially controlled stiffness changes and drive cell morphology through mechanical cues. Elastic modulus rises by more than double after photocross-linking, as shown by atomic force microscopy measurements. Biological response is also analyzed and stiffness-dependent cell spreading and proliferation are verified. Different pattern geometries are successfully realized by UV lithography, allowing 2D cross-linking modulation. Furthermore, 3D mechanical tuning at micro- and submicrometer scale by two-photon polymerization makes this system a biologically relevant matrix to study cell functions and tissue development.

Light-Mediated Manufacture and Manipulation of Actuators.

Recent years have seen a considerable growth of research interests in developing novel technologies that permit designable manufacture and controllable manipulation of actuators. Among various fabrication and driving strategies, light has emerged as an enabler to reach this end, contributing to the development of actuators. Several accessible light-mediated manufacturing technologies, such as ultraviolet (UV) lithography and direct laser writing (DLW), are summarized. A series of light-driven strategies including optical trapping, photochemical actuation, and photothermal actuation for controllable manipulation of actuators is introduced. Current challenges and future perspectives of this field are discussed. To generalize, light holds great promise for the development of actuators.

Large-Area High Aspect Ratio Plasmonic Interference Lithography Utilizing a Single High-k Mode.

Plasmonic lithography, which utilizes subwavelength confinement of surface plasmon polartion (SPP) waves, has the capability of breaking the diffraction limit and delivering high resolution. However, all previously reported results suffer from critical issues, such as shallow pattern depth and pattern nonuniformity even over small exposure areas, which limit the application of the technology. In this work, periodic patterns with high aspect ratios and a half-pitch of about 1/6 of the wavelength were achieved with pattern uniformity in square centimeter areas. This was accomplished by designing a special mask and photoresist (PR) system to select a single high spatial frequency mode and incorporating the PR into a waveguide configuration to ensure uniform light exposure over the entire depth of the photoresist layer. In addition to the experimental progress toward large-scale applications of plasmonic interference lithography, the general criteria of designing such an exposure system is also discussed, which can be used for nanoscale fabrication in this fashion for various applications with different requirements for wavelength, pitch, aspect ratio, and structure.

Deconstructing the Effects of Matrix Elasticity and Geometry in Mesenchymal Stem Cell Lineage Commitment.

A wide variety of environmental factors including physical and biochemical signals are responsible for stem cell behavior and function. In particular, matrix elasticity and cell shape have been shown to determine stem cell function, yet little is known about the interplay between how these physical cues control cell differentiation. For the first time, by using ultraviolet (UV) lithography to pattern poly(ethylene) glycol (PEG) hydrogels we are able to manufacture microenvironments capable of parsing the effects of matrix elasticity, cell shape, and cell size in order to explore the relationship between matrix elasticity and cell shape in mesenchymal stem cell (MSC) lineage commitment. Our data shows that cells cultured on 1,000 µm2 circles, squares, and rectangles were primarily adipogenic lineage regardless of matrix elasticity, while cells cultured on 2,500 and 5,000 µm2 shapes more heavily depended on shape and elasticity for lineage specification. We further went on to characterize how modifying the cell cytoskeleton through pharmacological inhibitors can modify cell behavior. By showing MSC lineage commitment relationships due to physical signals, this study highlights the importance of cell shape and matrix elasticity in further understanding stem cell behavior for future tissue engineering strategies.

Patterning of polymeric cell culture substrates.

The purpose of this chapter is to provide a summary of polymer patterning technologies for biological applications and detailed instructions for resist-free deep ultraviolet (UV) patterning of poly(styrene). Photochemical modifications of this polymer yield unstable peroxides together with stable oxidized chemical groups. The altered physicochemical properties of the polymer surface influence protein adsorption and cell adhesion. HepG2 (human hepatoma cell line), fibroblasts (L929, murine fibroblast line), and other cell lines exhibit strong adhesion on areas of UV-irradiated polymer. Masked irradiations open a simple, fast (cell patterns are obtained within a few hours), and economical route to obtain chemically patterned cell culture substrates. The described protocol is advantageous compared to silane-based patterning techniques on glass or thiol-based patterning on gold because of the elimination of any chemical treatment and the small size of achieved structures. The protocol is compatible with common clean room technologies; however, even without access to a clean room, structured substrates can be produced. The described technique can be a useful tool for a variety of cell cultures used to study biological processes like intercellular communication and organogenesis and for applications like biosensing or tissue engineering.

Fabrication of 3D Controlled in vitro Microenvironments.

Microfluidics-based lab-on-a-chips have many advantages, one of which is to provide physiologically relevant settings for cell biology experiments. Thus there is an ever increasing interest in their fabrication. Our goal is to construct three dimensional (3D) Controlled in vitro Microenvironments (CivMs) that mimic the in vivo microenvironments. Here, we present our optimized fabrication method that works for various lab-on-a-chip designs with a wide range of dimensions. The most crucial points are:•While using one type of SU-8 photoresist (SU-2075), fine tuning of ramp, dwell time, spin speed, durations of soft bake, UV exposure and development allows fabrication of SU-8 masters with various heights from 40 to 600 µm.•Molding PDMS (polydimethylsiloxane) at room temperature for at least two days instead of baking at higher temperatures prevents not only tears and bubbles in PDMS stamps but also cracks in the SU-8 master.•3D nature of the CivMs is ensured by keeping the devices inverted during gel polymerization.