Publications

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In this work, we investigate the linear optical response of a dielectric metasurface made of vertically-oriented germanium ellipses deposited on walls of a micron-scale cubic silicon nitride unit cell support matrix.

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A wall-first variant of membrane projection lithography (MPL) is introduced which yields three-dimensional meta-films; mm-scale structures with micron-scale periodicity and 3D nm-scale unit cell structure. These meta-films combine aspects of photonic crystals, metamaterials and plasmonic nano antennas in their infrared scattering behavior. We present the fabrication approach, and modeling/IR characterization results.

A complementary metal oxide semiconductor (CMOS) compatible fabrication method for creating three-dimensional (3D) meta-films is presented. In contrast to metasurfaces, meta-films possess structural variation throughout the thickness of the film and can possess a sub-wavelength scale structure in all three dimensions. Here we use this approach to create 2D arrays of cubic silicon nitride unit cells with plasmonic inclusions of elliptical metallic disks in horizontal and vertical orientations with lateral array-dimensions on the order of millimeters. Fourier transform infrared (FTIR) spectroscopy is used to measure the infrared transmission of meta-films with either horizontally or vertically oriented ellipses with varying eccentricity. Shape effects due to the ellipse eccentricity, as well as localized surface plasmon resonance (LSPR) effects due to the effective plasmonic wavelength are observed in the scattering response. The structures were modeled using rigorous coupled wave analysis (RCWA), finite difference time domain (Lumerical), and frequency domain finite element (COMSOL). The silicon nitride support structure possesses a complex in-plane photonic crystal slab band structure due to the periodicity of the unit cells. We show that adjustments to the physical dimensions of the ellipses can be used to control the coupling to this band structure. The horizontally oriented ellipses show narrow, distinct plasmonic resonances while the vertically oriented ellipses possess broader resonances, with lower overall transmission amplitude for a given ellipse geometry. We attribute this difference in resonance behavior to retardation effects. The ability to couple photonic slab modes with plasmonic inclusions enables a richer space of optical functionality for design of metamaterial-inspired optical components.

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In this paper we present a design concept for 3D plasmonic scatterers as high-efficiency transmissive metasurface (MS) building blocks. A genetic algorithm (GA) routine partitions the faces of the walls inside an open cavity into a M x N grid of voxels which can be either covered with metal or left bare, and optimizes the distribution of metal coverage needed to generate electric and magnetic modes of equal strength with a targeted phase delay (Φt) at the design wavelength. Even though the electric and magnetic modes can be more complicated than typical low order modes, with their spectral overlap and equal strengths, they act as a Huygens source, with the accompanying low reflection magnitude. Square/hexagonal voxels inside square/rectangular cavities are thoroughly analyzed for operation at 8 µm, although the technique can be applied to different cavity geometries for operation across the electromagnetic spectrum. Results from full-wave simulations show the GA routine can repeatedly pinpoint scatterer geometries emitting at any Φt value across 2π phase space with transmittances of at least 60%, making these MS building blocks an attractive plasmonic alternative for practical optical applications. Full-scale metasurface devices are calculated from near-fields of the individual elements to validate the optical functionality.

Metamaterials research has developed perfect absorbers from microwave to optical frequencies, mainly featuring planar metamaterials, also referred to as metasurfaces. In this study, we investigated vertically oriented metamaterials, which make use of the entire three-dimensional space, as a new avenue to widen the spectral absorption band in the infrared regime between 20 and 40 THz. Vertically oriented metamaterials, such as those simulated in this work, can be experimentally realized through membrane projection lithography, which allows a single unit cell to be decorated with multiple resonators by exploiting the vertical dimension. In particular, we analyzed the cases of a unit cell containing a single vertical split-ring resonator (VSRR), a single planar split-ring resonator (PSRR), and both a VSRR and PSRR to explore intra-cell coupling between resonators. We show that the additional degrees of freedom enabled by placing multiple resonators in a unit cell lead to novel ways of achieving omnidirectional super absorption. Our results provide an innovative approach for controlling and designing engineered nanostructures.

Membrane projection lithography (MPL) is a fabrication approach in which a novel process flow and mature silicon processing equipment combine to create three-dimensional metamaterials with size scales operational at optical frequencies. In its most common realization, MPL leverages microelectromechanical (MEMS) processing techniques to create cubic unit cells with silicon walls, planarized by chemical mechanical polishing (CMP), a technique that is not omnipresent in fabrication facilities. Here we show several variants of MPL, two of which do not require CMP to make the MPL process compatible with low-tech fabrication environments and open the MPL process to a wider audience.

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Control and manipulation of polarisation is an important topic for imaging and light matter interactions. In the infrared regime, the large wavelengths make wire grid polarisers (WGPs) a viable option, as it is possible to create periodic arrays of metallic wires at that scale. The recent advent of metamaterials has spurred an increase in non-traditional polariser motifs centred around more complicated repeat units, which potentially provide more functionality. The authors explore the use of 2D arrays of single and back-to-back vertically oriented cross dipoles arranged in a cubic in-plane silicon matrix. They show that both single and back-to-back versions have higher rejection ratios and larger bandwidths than either WGPs or 2D arrays of linear dipoles.

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Metamaterials provide a means to tailor the spectral response of a surface. Given the periodic nature of the metamaterial, proper design of the unit cell requires intimate knowledge of the parameter space for each design variable. We present a detailed study of the parameter space surrounding vertical split-ring resonators and planar split-ring resonators, and demonstrate widening of the perfect absorption bandwidth based on the understanding of its parameter space.

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Three-dimensional (3D) metafilms composed of periodic arrays containing single and multiple micrometer-scale vertical split ring resonators per unit cell were fabricated using membrane projection lithography. In contrast to planar and stacked planar structures such as cut wire pairs and fishnet structures, these 3D metafilms have a thickness t ∼λd/4, allowing for classical thin film effects in the long wavelength limit. The infrared specular far-field scattering response was measured for metafilms containing one and two resonators per unit cell, and compared to numerical simulations. Excellent agreement in the frequency region below the onset of diffractive scattering was obtained. The metafilms demonstrate strong bi-anisotropic polarization dependence. Further, we show that for 3D metafilms, just as in solids, complex unit cells with multiple atoms (inclusions) per unit cell possess a richer set of excitation mechanisms. The highlight of these new coupling mechanisms is the excitation of the 3D analog to the 2D cut-wire-pair magnetic response.

The manufacturing tolerances of a stencil-lithography variant, membrane projection lithography, were investigated. In the first part of this work, electron beam lithography was used to create stencils with a range of linewidths. These patterns were transferred into the stencil membrane and used to pattern metallic lines on vertical silicon faces. Only the largest lines, with a nominal width of 84 nm, were resolved, resulting in 45 ± 10 nm (average ± standard deviation) as deposited with 135-nm spacing. Although written in the e-beam write software file as 84-nm in width, the lines exhibited linewidth bias. This can largely be attributed to nonvertical sidewalls inherent to dry etching techniques that cause proportionally larger impact with decreasing feature size. The line edge roughness can be significantly attributed to the grain structure of the aluminum nitride stencil membrane. In the second part of this work, the spatial uniformity of optically defined (as opposed to e-beam written) metamaterial structures over large areas was assessed. A Fourier transform infrared spectrometer microscope was used to collect the reflection spectra of samples with optically defined vertical split ring from 25 spatially resolved 300 × 300 μm regions in a 1-cm2 area. The technique is shown to provide a qualitative measure of the uniformity of the inclusions.

This paper investigates three-dimensional cut wire pair (CWP) behavior in vertically oriented meta-atoms. We first analyze CWP metamaterial inclusions using full-wave electromagnetic simulations. The scattering behavior of the vertical CWP differs substantially from that of the planar version of the same structure. In particular, we show that the vertical CWP supports a magnetic resonance that is solely excited by the incident magnetic field. This is in stark contrast to the bianisotropic resonant excitation of in-plane CWPs. We further show that this CWP behavior can occur in other vertical metamaterial resonators, such as back-to-back linear dipoles and back-to-back split ring resonators (SRRs), due to the strong coupling between the closely spaced metallic elements in the back-to-back configuration. In the case of SRRs, the vertical CWP mode (unexplored in previous literature) can be excited with a magnetic field that is parallel to both SRR loops, and exists in addition to the familiar fundamental resonances of the individual SRRs. In order to fully describe the scattering behavior from such dense arrays of three-dimensional structures, coupling effects between the close-packed inclusions must be included. The new flexibility afforded by using vertical resonators allows us to controllably create purely electric inclusions, purely magnetic inclusions, as well as bianisotropic inclusions, and vastly increases the degrees of freedom for the design of metafilms.

Structured electromagnetic materials have experienced a renaissance with the emergence of metamaterial and plasmonic research. The ability to orient metallic plasmonic inclusions vertically enables orientation-dependent coupling arrangements which cannot be achieved in conventional planar engineered materials. In this paper we discuss these coupling arrangements and their effect on the measured far field scattering response to normally incident excitation.

Three-dimensional (3D) metafilms composed of periodic arrays of silicon unit cells containing single and multiple micrometer-scale vertical split ring resonators (SRRs) per unit cell were fabricated. In contrast to planar and stacked planar structures, these 3D metafilms have a thickness t ∼ λd/4, allowing for classical thin film effects in the long wavelength limit. The infrared specular far-field scattering response was measured for metafilms containing one and two resonators per unit cell and compared to numerical simulations. Excellent agreement in the frequency region below the onset of diffractive scattering was obtained. For dense arrays of unit cells containing single SRRs, normally incident linearly polarized plane waves which do not excite a resonant response result in thin film interference fringes in the reflected spectra and are virtually indistinguishable from the scattering response of an undecorated array of unit cells. For the resonant linear polarization, the specular reflection for arrays is highly dependent on the SRR orientation on the vertical face for gap-up, gap-down, and gap-right orientations. For dense arrays of unit cells containing two SRRs per unit cell positioned on adjacent faces, the specular reflection spectra are slightly modified due to near-field coupling between the orthogonally oriented SRRs but otherwise exhibit reflection spectra largely representative of the corresponding single-SRR unit cell structures. The ability to pack the unit cell with multiple inclusions which can be independently excited by choice of incident polarization suggests the construction of dual-channel films where the scattering response is selected by altering the incident polarization.

Lead halide perovskites are increasingly considered for applications beyond photovoltaics, for example, light emission and detection, where an ability to pattern and prototype microscale geometries can facilitate the incorporation of this class of materials into devices. Here we demonstrate laser direct write of lead halide perovskites, a remarkably simple procedure that takes advantage of the inverse dependence between perovskite solubility and temperature by using a laser to induce localized heating of an absorbing substrate. We demonstrate arbitrary pattern formation of crystalline CH3NH3PbBr3 on a range of substrates and fabricate and characterize a microscale photodetector using this approach. This direct write methodology provides a path forward for the prototyping and production of perovskite-based devices.

A method for patterning on vertical silicon surfaces in high aspect ratio silicon topography is presented. A Faraday cage is used to direct energetic reactive ions obliquely through a patterned suspended membrane positioned over the topography. The technique is capable of forming high-fidelity pattern (100 nm) features, adding an additional fabrication capability to standard top-down fabrication approaches.

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This paper demonstrates that another class of three-dimensional integrated circuits (3D-ICs) exists, distinct from through silicon via centric and monolithic 3D-ICs. Furthermore, it is possible to create devices that are 3D at the device level (i.e. with active channels oriented in each of the three coordinate axes), by performing standard CMOS fabrication operations at an angle with respect to the wafer surface into high aspect ratio silicon substrates using membrane projection lithography (MPL). MPL requires only minimal fixturing changes to standard CMOS equipment, and no change to current state-of-the-art lithography. Eliminating the constraint of 2D planar device architecture enables a wide range of new interconnect topologies which could help reduce interconnect resistance/capacitance, and potentially improve performance.

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The magnetostatic response of a variety of 3D metallic loop traces are studied numerically by evaluating the Biot- Savart law as a first step in understanding the radiative behavior of such structures. These numerical studies confirm that the magnetostatic behavior of localized planar and non-planar current distributions are equivalent to magnetic dipoles in the far field, however the near-field behavior of these traces can be quite different. © 2012 SPIE.

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The advancement of materials technology towards the development of novel 3D nanostructures for energy applications has been a long-standing challenge. The purpose of this project was to explore photolithographically defineable pyrolyzed photoresist carbon films for possible energy applications. The key attributes that we explored were as follows: (1) Photo-interferometric fabrication methods to produce highly porous (meso, micro, and nano) 3-D electrode structures, and (2) conducting polymer and nanoparticle-modification strategies on these structures to provide enhanced catalytic capabilities and increase conductivity. The resulting electrodes were then explored for specific applications towards possible use in battery and energy platforms.

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Metamaterials form a new class of artificial electromagnetic materials that provides the device designer with the ability to manipulate the flow of electromagnetic energy in ways that are not achievable with naturally occurring materials. However, progress toward practical implementation of metamaterials, particularly at infrared and visible frequencies, has been hampered by a combination of absorptive losses; the narrow band nature of the resonant metamaterial response; and the difficulty in fabricating fully 3-dimensional structures. They describe the progress of a recently initiated program at Sandia National Laboratories directed toward the development of practical 3D metamaterials operating in the thermal infrared. They discuss their analysis of fundamental loss limits for different classes of metamaterials. In addition, they discuss new design approaches that they are pursuing which reduce the reliance on metallic structures in an effort to minimize ohmic losses.

We present a new fabrication technique called Membrane Projection Lithography for the production of three-dimensional metamaterials at infrared wavelengths. Using this technique, multilayer infrared metamaterials that include both in-plane and out-of-plane resonators can be fabricated.

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The authors have developed two versions of a flexible fabrication technique known as membrane projection lithography that can produce nearly arbitrary patterns in '212 D' and fully three-dimensional (3D) structures. The authors have applied this new technique to the fabrication of split ring resonator-based metamaterials in the midinfrared. The technique utilizes electron beam lithography for resolution, pattern design flexibility, and alignment. The resulting structures are nearly three orders of magnitude smaller than equivalent microwave structures that were first used to demonstrate a negative index material. The fully 3D structures are highly isotropic and exhibit both electrically and magnetically excited resonances for incident transverse electromagnetic waves.

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This senior council Tier 1 LDRD was focused on exploring the use of porous growth masks as a method for defect reduction during heteroepitaxial crystal growth. Initially our goal was to investigate porous silica as a growth mask, however, we expanded the scope of the research to include several other porous growth masks on various size scales, including mesoporous carbon, photolithographically patterned SU-8 and carbonized SU-8 structures. Use of photolithographically defined growth templates represents a new direction, unique in the extensive literature of patterned epitaxial growth, and presents the possibility of providing a single step growth mask. Additional research included investigation of pore viability via electrochemical deposition into high aspect ratio photoresist. This project was a small footprint research effort which, nonetheless, produced significant progress towards both the stated goal as well as unanticipated research directions.

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This one-year out-of-the-box LDRD was focused on exploring the use of porous growth masks as a method for defect reduction during heteroepitaxial crystal growth. Initially our goal was to investigate porous silica as a growth mask, however, we expanded the scope of the research to include several other porous growth masks on various size scales, including mesoporous carbon, and the UV curable epoxy, SU-8. Use of SU-8 as a growth mask represents a new direction, unique in the extensive literature of patterned epitaxial growth, and presents the possibility of providing a single step growth mask. Additional research included investigation of pore viability via electrochemical deposition into high aspect ratio photoresist patterns and pilot work on using SU-8 as a DUV negative resist, another significant potential result. While the late start nature of this project pushed some of the initial research goals out of the time table, significant progress was made. 3 Acknowledgements This work was performed in part at the Nanoscience @ UNM facility, a member of the National Nanotechnology Infrastructure Network, which is supported by the National Science Foundation (Grant ECS 03-35765). Sandia is multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United Stated Department of Energy's National Nuclear Security Administration under Contract DE-AC04-94AL85000. This work was supported under the Sandia LDRD program (Project 99405). 4

A gecko's extraordinary ability to suspend itself from walls and ceilings of varied surface roughness has interested humans for hundreds of years. Many theories and possible explanations describing this phenomenon have been proposed including sticky secretions, microsuckers, and electrostatic forces; however, today it is widely accepted that van der Waals forces play the most important role in this type of dry adhesion. Inarguably, the vital feature that allows a gecko's suspension is the presence of billions 3 of tiny hairs on the pad of its foot called spatula. These features are small enough to reach within van der Waals distances of any surface (spatula radius %7E100 nm); thus, the combined effect of billions of van der Waals interactions is more than sufficient to hold a gecko's weight to surfaces such as smooth ceilings or wet glass. Two lithographic approaches were used to make hierarchal structures with dimensions similar to the gecko foot dimensions noted above. One approach combined photo-lithography with soft lithography (micro-molding). In this fabrication scheme the fiber feature size, defined by the alumina micromold was 0.2 um in diameter and 60 um in height. The second approach followed more conventional photolithography-based patterning. Patterned features with dimensions %7E0.3 mm in diameter by 0.5 mm tall were produced. We used interfacial force microscopy employing a parabolic diamond tip with a diameter of 200 nm to measure the surface adhesion of these structures. The measured adhesive forces ranged from 0.3 uN - 0.6 uN, yielding an average bonding stress between 50 N/cm2 to 100 N/cm2. By comparison the reported literature value for the average stress of a Tokay gecko foot is 10 N/cm2. Acknowledgements This work was funded by Sandia National Laboratory's Laboratory Directed Research & Development program (LDRD). All coating processes were conducted in the cleanroom facility located at the University of New Mexico's Center for High Technology Materials (CHTM). SEM images were performed at UNM's Center for Micro-Engineering on equipment funded by a NSF New Mexico EPSCoR grant. 4

Our discovery that the introduction of living cells (Saccharomyces cerevisiae) alters dramatically the evaporation driven self-assembly of lipid-silica nanostructures suggested the formation of novel bio/nano interfaces useful for cellular interrogation at the nanoscale. This one year ''out of the box'' LDRD focused on the localization of metallic and semi-conducting nanocrystals at the fluid, lipid-rich interface between S. cerevisiae and the surrounding phospholipid-templated silica nanostructure with the primary goal of creating Surface Enhanced Raman Spectroscopy (SERS)-active nanostructures and platforms for cellular integration into electrode arrays. Such structures are of interest for probing cellular responses to the onset of disease, understanding of cell-cell communication, and the development of cell-based bio-sensors. As SERS is known to be sensitive to the size and shape of metallic (principally gold and silver) nanocrystals, various sizes and shapes of nanocrystals were synthesized, functionalized and localized at the cellular surface by our ''cell-directed assembly'' approach. Laser scanning confocal microscopy, SEM, and in situ grazing incidence small angle x-ray scattering (GISAXS) experiments were performed to study metallic nanocrystal localization. Preliminary Raman spectroscopy studies were conducted to test for SERS activity. Interferometric lithography was used to construct high aspect ratio cylindrical holes on patterned gold substrates and electro-deposition experiments were performed in a preliminary attempt to create electrode arrays. A new printing procedure was also developed for cellular integration into nanostructured platforms that avoids solvent exposure and may mitigate osmotic stress. Using a different approach, substrates comprised of self-assembled nanoparticles in a phospholipid templated silica film were also developed. When printed on top of these substrates, the cells integrate themselves into the mesoporous silica film and direct organization of the nanoparticles to the cell surface for integration into the cell.