Scalable Fabrication of 4 nm Silicon Nanopores by Self-Limiting Metal-Assisted Chemical Etching Combined with Optical Process Control.

Solid-state nanopores in ultrathin (<20 nm) membranes enable label-free single-molecule sensing, but their adoption as sensors is limited by the lack of scalable manufacturing methods that deliver nanopores with single-nanometer reproducibility. Self-limiting metal-assisted chemical etching (MACE) in silicon-on-insulator (SOI) membranes offers a parallel wet-chemical route for nanopore fabrication, yet prior demonstrations lacked a predictive design rule and required electron microscopy or electrical tests for confirming presence and number of pores. Here, we convert self-limiting MACE into a manufacturing-oriented workflow with optical process control to obtain and verify the formation of 4 nm nanopores in a scalable fashion. We decouple the deposition of 200 ± 10 nm gold (Au) nanoparticles from etching, enabling independent optimization of the two steps. The nanoparticle size allows for particle-per-membrane counting by dark-field optical microscopy, so that deposition can be repeated when counts are below target. We then map etching behavior across Au nanoparticle diameter