Characterization of tin selenides synthesized by high-energy milling
Tin selenides SnSeX (x=1,2) were synthesized from tin and selenium powder precursors by high-energy milling in the planetary ball mill Pulverisette 6 (Fritsch, Germany). The orthorhombic tin selenide SnSe and the hexagonal tin diselenide SnSe2 phases were formed after 4 min and 5 min of milling, respectively. Specific surface area of both selenides increased with increasing time of mechanochemical synthesis. The particle size distribution analysis demonstrated that the synthesized products contain agglomerated selenide particles consisting of numerous idiomorphic tin selenide crystals, measuring from 2 to more than 100 nm in diameter, which were also documented by TEM. UV-Vis spectrophotometry confirmed that tin selenide particles do not behave as quantum dots.
Characterization of mechanochemically synthesized lead selenide
Mechanochemical synthesis of lead selenide PbSe nanocrystals was performed by high-energy milling of lead and selenium powders in a planetary ball mill. The structure properties of synthesized lead selenide were characterized by XRD analysis that confirmed crystalline nature of PbSe nanocrystals. Calculated average size of PbSe crystallites was 37 nm. The methods of particle size distribution analysis, specific surface area measurement, SEM and TEM were used for the characterization of surface and morphology of PbSe nanocrystals. SEM analysis revealed agglomerates of PbSe particles. However, HRTEM analysis confirmed perfect stoichiometric PbSe cubes with NaCl structure as well. UV-VIS-NIR spectrophotometry was used to confirm the blue shift of the small particles occurring in the powder product obtained by the mechanochemical synthesis.
Effects of the mineral phase and valence of vanadium on vanadium extraction from stone coal
The influence of roasting on the leaching rate and valence of vanadium was evaluated during vanadium extraction from stone coal. Vanadium in stone coal is hard to be leached and the leaching rate is less than 10% when the raw ore is leached by 4 mol/L H2SO4 at 90°C for 2 h. After the sample is roasted at 900°C for 2 h, the leaching rate of vanadium reaches the maximum, and more than 70% of vanadium can be leached. The crystal of vanadium-bearing mica minerals decomposes and the content of V(V) increases with the rise of roasting temperature from 600 to 900°C, therefore the leaching rate of vanadium increases significantly with the decomposition of the mica minerals. Some new phases, anorthite for example, form when the roasting temperature reaches 1000°C. A part of vanadium may be enwrapped in the sintered materials and newly formed phases, which may impede the oxidation of low valent vanadium and make the leaching rate of vanadium drop dramatically. The leaching rate of vanadium is not only determined by the valence state of vanadium but also controlled by the decomposition of vanadium-bearing minerals and the existence state of vanadium to a large extent.