Crystalline gallium (III) sulfide Ga 2 S 3 samples have been prepared by mechanical-alloying instead of usual heating process. A safe, energy-efficient, and fast process of only 4 hours of mechanosynthesis led to the formation of polycrystalline Ga 2 S 3 from pure Ga and S as raw materials. X-ray diffraction measurements and Rietveld refinements show that the as-prepared material is a mixture of mainly hexagonal wurtzite-type β-phase (68 ± 5 wt%; space group P6 3 mc (No. 186)) along with some cubic sphalerite-type γ-phase (32 ± 5 wt%; space group F-43m (No. 216)). In situ high-temperature X-ray diffraction measurements show that the monoclinic phase (space group Cc (No. 9)) appears at 450°C. Scanning electron microscopy analyses reveal that the morphology of the powder is characterized by aggregates of nanometric *Revised Manuscript (corrections hidden) Click here to download Revised Manuscript (corrections hidden): Papier_Ga2S3_revision_without_highlights.docx particles. Their sizes measured by laser diffraction show a median size around 170 nm after 4 hours of ball-milling.
NaGaS2 is a newly discovered compound that
has already
shown great promise for a variety of applications because of its layered
structure and ion exchange properties. In this work, crystalline NaGaS2 has been synthesized by an alternative method to what has
been previously published, namely, by mechanochemistry, either by
a direct one-step process or by a two-step process. In the one-step
process, crystalline NaGaS2 is directly formed by milling
sodium sulfide Na2S and gallium(III) sulfide Ga2S3. However, an amorphous material is present in majority
together with the crystalline phase. In the two-step process, amorphous
NaGaS2 is first obtained by mechanical milling and then
heated above its glass transition temperature to obtain a glass–ceramic
mainly composed of crystalline NaGaS2. For the two-step
process, changes of the local atomic-level structure in amorphous
NaGaS2 and after crystallization were analyzed by high-field
solid-state nuclear magnetic resonance (NMR) spectroscopy as well
as by X-ray total scattering and pair distribution function (PDF)
analysis. Based on quantitative analysis on the 23Na NMR
spectra, modifying the annealing treatment can promote the formation
of the crystalline phase up to a molar fraction of 83.8%.
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