Optimization of HNA etching parameters to produce high aspect ratio solid silicon microneedles

Abstract

High aspect ratio solid silicon microneedles with a concave conic shape were fabricated. Hydrofluoric acid–nitric acid–acetic acid (HNA) etching parameters were characterized and optimized to produce microneedles that have long and narrow bodies with smooth surfaces, suitable for transdermal drug delivery applications. The etching parameters were characterized by varying the HNA composition, the optical mask's window size, the etching temperature and bath agitation. An L9 orthogonal Taguchi experiment with three factors, each having three levels, was utilized to determine the optimal fabrication parameters. Isoetch contours for HNA composition with 0% and 10% acetic acid concentrations were presented and a high nitric acid region was identified to produce microneedles with smooth surfaces. It is observed that an increase in window size indiscriminately increases the etch rate in both the vertical and lateral directions, while an increase in etching temperature beyond 35 °C causes the etching to become rapid and uncontrollable. Bath agitation and sample placement could be manipulated to achieve a higher vertical etch rate compared to its lateral counterpart in order to construct high aspect ratio microneedles. The Taguchi experiment performed suggests that a HNA composition of 2:7:1 (HF:HNO3:CH3COOH), window size of 500 µm and agitation rate of 450 RPM are optimal. Solid silicon microneedles with an average height of 159.4 µm, an average base width of 110.9 µm, an aspect ratio of 1.44, and a tip angle and diameter of 19.2° and 0.38 µm respectively were successfully fabricated.