Fabrication of Sb₂S₃ Thin Films by Low-Temperature Plasma-Sulfurizing Metallic Sb Layers

Abstract

In this work, antimony sulfide (Sb2S3) thin films were prepared by low-temperature plasma (about 190 °C) sulfidation of antimony metal layers, and the sulfidation mechanism was investigated. Solid sulfur powder was used as the sulfur source, and the reaction process did not exhaust toxic gases. The relevant process parameters, including the reaction pressure, radio frequency (RF) power, and sulfurization time, were also optimized. Under conditions of an RF power of 180 W (approximately 190 °C), a curing time of 60 min, and a working pressure of 30 Pa, we prepared a smooth, pinhole-free, (211) preferentially oriented Sb2S3 thin film. The film obtained good photocurrent response and a suitable band gap of 1.74 eV. The properties and structures of the Sb2S3 thin film were characterized by optical emission spectroscopy, high-resolution scanning electron microscopy, energy-dispersive spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and UV and Raman spectroscopies.

Influence of Sulfurization Time on Sb2S3 Synthesis Using a New Graphite Box Design

“…However, after Sb thin film sulfurization, an important change in grain shape and distribution can be observed (Figure 4io). The film thicknesses range from 0.4 to 1.7 µm; such a large thickness variation is a consequence of recrystallization and the Sb2S3 formation, as J. Zhang suggests [14]. The qualitative analysis using EDS lines confirms the sulfur diffusion through the Sb thin film in all the samples.…”

“…The method proposed (two-step process and graphite box) in this work is effective for Sb 2 S 3 formation. On the other hand, after sulfurization at 20 min, it was possible to identify small peaks related to metallic Sb peaks, indicating that the sample has not been wholly sulfurized and probably recrystallized [11][12][13][14]. However, these peaks' intensity decreases as the time increases to 30 and 40 min, while at 50 min, the Sb peak shows a slight increase in intensity.…”

“…The previous work that implemented a two-step process includes the one presented by Lei et al [13], who deposited metallic Sb by RF-sputtering with a subsequent in situ hydrothermal process to Materials 2024, 17, 1656 2 of 12 obtain Sb 2 S 3 . Additionally, L. Zhang et al deposited metallic Sb thin films using the TE method and performed annealing in nitrogen/hydrogen sulfide (N 2 /H 2 S) atmosphere to form Sb 2 S 3 [12]; while J. Zhang et al obtained Sb 2 S 3 by low-temperature plasma sulfurizing metallic Sb using sulfur powder varying the radiofrequency power conditions [14].…”

Low‐Temperature Vapor‐Phase Growth of 2D Metal Chalcogenides

“…[79,80] In addition to the PI substrate, the MoS 2 film was also deposited onto regular microscopic glass substrates (Figure 4b) by a similar PECVD strategy for transparent thin film transistor (TFT) and phototransistor applications. Beyond the growth of MoS 2 , the plasmaassisted metal chalcogenization process is also applicable for synthesizing various 2D chalcogenides at low temperature, such as WSe 2 , [81] PtSe 2 , [82] PdSe 2 , [83] Sb 2 S 3 , [84] 1T-WS 2 , [85] etc, and their resulting thickness can be tuned by the initially deposited metal film thickness. Moreover, this method has been extended to directly synthesize large-scale MoS 2 -WS 2 vertical heterostructures at a low temperature (300 °C).…”