Antimonene, a novel group 15 two-dimensional material, is attracting great attention due to its outstanding physical and chemical properties. Despite its thermodynamic stability, the pronounced covalent character of the interlayer interactions imposes severe limitations on its exfoliation into mono- and few-layer. Here, we develop a systematic study of liquid phase exfoliation (LPE) with the aim to optimize antimonene production in terms of concentration and dimensional anisotropy, investigating the most relevant experimental factors affecting the exfoliation: pre-processing of pristine antimony, solvent selection based on Hansen solubility parameters and ultrasound conditions. Moreover, exhaustive characterization by means of turbidimetry, XRD, Raman spectroscopy, XPS, AFM, SEM, XEDS and TEM has been carried out. Indeed, we achieved concentration values of ca. 0.368 g L⁻¹ (∼yield of 37 wt%), up to ∼30 times higher compared to the highest value so far reported, with ca. 50% of the nanolayers with heights between 2 and 10 nm and lateral dimensions in the 40–300 nm range. Furthermore, it has been demonstrated that the yield of the process can be enhanced up to ∼90 wt% by recycling the sediment to perform a maximum of 7 cycles. Moreover, we have illustrated the usefulness of this approach by characterizing the electrochemical behaviour of antimonene as a catalyst for the hydrogen evolution reaction (HER). This study provides important insights into the LPE and electrochemical properties of antimonene, allowing its large-scale production and paving the way for its application in fields of utmost importance such as energy storage and conversion or catalysis.

Antimonene, a monolayer of β-antimony, is increasingly attracting considerable attention, more than that of other monoelemental two-dimensional materials, due to its intriguing physical and chemical properties. Under ambient conditions, antimonene exhibits a high thermodynamic stability and good structural integrity. Some theoretical calculations predicted that antimonene would have a high oxidation tendency. However, it remains poorly investigated from the experimental point of view. In this work, we study the oxidation behavior of antimonene nanosheets (ANS) prepared by ultrasonication-assisted liquid-phase exfoliation. Using a set of forefront analytical techniques, a clear effect of sonication time on the surface chemistry of prepared ANS is found. A dynamic oxidation behavior has been observed, which upon annealing at moderate temperature (210 °C) resulted in a semiconducting behavior with a bandgap of approximately 1 eV measured by ultraviolet photoelectron spectroscopy. This study yields valuable information for future applications of antimonene and paves the way towards novel modification approaches in order to tailor its properties and complement its limitations.

Two-dimensional (2D) antimony, so-called antimonene, can form antimonene oxide when exposed to air. We present different types of single- and few-layer antimony oxide structures, based on density functional theory (DFT) calculations. Depending on stoichiometry and bonding type, these novel 2D layers have different structural stability and electronic properties, ranging from topological insulators to semiconductors with direct and indirect band gaps between 2.0 and 4.9 eV. We discuss their vibrational properties and Raman spectra for experimental identification of the predicted structures.

Two-dimensional (2D) sheets of antimonene have attracted increasing attention due to their unique physical and chemical properties prompting potential for diverse applications. We present a facile method to prepare high-quality antimonene nanosheets (ANSs) by micromechanical exfoliation on SiO₂/Si substrate. The temperature- and laser power-dependent Raman studies of exfoliated ANSs are reported and analyzed. It was found that both the out-of-plane A_1g and the in-plane E_g modes red-shift linearly with increase in temperature, pointing towards anharmonic vibrations of the lattice. The thermal response of the ANSs on a SiO₂/Si surface is also described using numerical simulation of the heat transfer to study their laser-induced oxidation mechanisms. These results offer a deeper understanding of the phonon properties and oxidation susceptibility of 2D antimonene paving the way for the development of antimonene-based technologies, such as electronic devices or photothermal cancer therapy.