The semiconductor industry’s transition to three-dimensional (3D) logic and memory devices has revealed the limitations of plasma etching in reliable creation of vertical high aspect ratio (HAR) nanostructures. Metal-assisted chemical etch (MacEtch) can create ultra-HAR, taper-free nanostructures in silicon, but the catalyst used for reliable MacEtchgoldis not CMOS (complementary metal–oxide–semiconductor)-compatible and therefore cannot be used in the semiconductor industry. Here, for the first time, we report a ruthenium MacEtch process that is comparable in quality to gold MacEtch. We introduce new process variablescatalyst plasma pretreatment and surface areato achieve this result. Ruthenium is particularly desirable as it is not only CMOS-compatible but has also been introduced in semiconductor fabrication as an interconnect material. The results presented here remove a significant barrier to adoption of MacEtch for scalable fabrication of 3D semiconductor devices, sensors, and biodevices that can benefit from production in CMOS foundries.

Modern high-throughput nanopatterning techniques, such as nanoimprint lithography, make it possible to fabricate arrays of nanostructures (features with dimensions of 10’s to 100’s of nm) over large area substrates (cm2 to m2 scale) such as Si wafers, glass sheets, and flexible roll-to-roll webs. The ability to make such large-area nanostructure arrays (LNAs) has created an extensive design space, enabling a wide array of applications including optical devices, such as wire-grid polarizers, transparent conductors, color filters, and anti-reflection surfaces, and building blocks for electronic components, such as ultracapacitors, sensors, and memory storage architectures. However, existing metrology methods will have trouble scaling alongside fabrication methods. Scanning electron microscopy (SEM) and atomic force microscopy (AFM), for instance, have micron scale fields of view (FOV) that preclude comprehensive characterization of LNAs, which may be manufactured at m2 per minute rates. Scatterometry approaches have larger FOVs (typically 100’s of µm to a few mm), but traditional scatterometry systems measure samples one point at a time, which also makes them too slow for large-scale LNA manufacturing. In this work, we demonstrate parallelization of the traditional spectroscopic scatterometry approach using hyperspectral imaging, increasing the throughput of the technique by a factor of 106-107. We demonstrate this approach by using hyperspectral imaging and inverse modeling of reflectance spectra to derive 3-dimensional geometric data for Si nanopillar array structures over both mm and cm-scale with µm-scale spatial resolution. This work suggests that geometric measurements for a variety of LNAs can be performed with the potential for high speed over large areas which may be critical for future LNA manufacturing.

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Metal Assisted Chemical Etching (MacEtch) of silicon shows reliable vertical anisotropic wet etching only in single-crystal silicon, which limits its applications to a small number of devices. This work extends the capabilities of MacEtch to polysilicon which has potential to enable high-volume and cost-sensitive applications such as optical metasurfaces, anodes for high capacity and flexible batteries, electrostatic supercapacitors, sensors, nanofluidic deterministic lateral displacement devices, etc. This work presents a MacEtch of polysilicon that produces nanostructure arrays with sub-50nm resolution and anisotropic profile. The three demonstrated structures are pillars of 5:1 aspect ratio and 50nm spacing for comparison to single crystal silicon MacEtch literature, pillars of 30nm spacing and a diamond pillar array with sharp corners to establish resolution limits of polysilicon MacEtch.