Precipitated ammonium aluminium carbonate hydroxide (NH4Al(OH)2CO3) is a promising precursor for preparation of nanostructured Al2O3. However, the experimental conditions, such as the low concentration of Al3+ salt solution, high temperature and/or pressure, long reaction time, and excessive amount of the (NH4)2CO3 precipitating agent, make this process expensive for large-scale production. Here, we report a simpler and cheaper route to prepare nanostructured alumina by partial neutralisation of a nearly saturated aqueous solution of Al(NO3)3 with (NH4)2CO3 as a base at pH < 4. Synthesis in the acidic region led to formation of a polynuclear aluminium cluster (Al13), which is an important “green” solution precursor for large-area preparation of Al2O3 thin films and nanoparticles. Control of the textural properties of the final alumina product during calcination of the prepared aluminium (oxy)hydroxide gel was accomplished by adding low-solubility aluminium acetate hydroxide (Al(OH)(CH3COO)2) as a seed to the Al(NO3)3 solution before neutralisation. The large Brunauer–Emmett–Teller specific surface area (376 m2 g−1) and narrow pore size distribution (2–20 nm) of the prepared compact alumina suggest that the chelating effect of the acetate ions affects the structures of the forming transition aluminas, and the evolved gases produced by decomposition of Al(OH)(CH3COO)2 and NH4NO3 as a by-product of the reaction during calcination prevent particle agglomeration. Other advantages of the proposed process are its versatility and the ability to obtain high purity materials without producing large amounts of by-products without the need for washing and energy saving by using a low processing temperature, and the possibility of recycling the generated CO2 and NH3 gases as the (NH4)2CO3 reagent.
23 June 2016 in Mineral Processing and Extractive Metallurgy Review
This study demonstrates an efficient synthesis of highly reactive silica using hydrometallurgical processing of serpentinite tailings. Proposed process uses two-stage (acid and alkaline) leaching of serpentinite tailings and precipitation of silica from the sodium metasilicate solution using hydrochloric acid. The alkaline leaching and the effect of impurities on the precipitation of amorphous silica under the conditions of maximum sol stability were examined in detail. The proposed route is technologically advantageous because the product did not contain residues of the original raw serpentinite and was characterized by high purity (99.4 wt. % SiO2), large specific area (541 m2 g–1), and consistent quality. Moreover, less sensitivity to the presence of impurities and longer gelation times, offering a longer time period for manipulating the product in the final stages of the process, were achieved. The total yield of silicon in the overall process was 90–91%.
A laboratory method was designed and verified that allows for the testing of alkaline, magnesite-based reactive materials for permeable reactive barriers (PRBs) to remove heavy metals from contaminated groundwater. It was found that caustic calcined magnesia (CCM) with high reactivity and low solubility to remove Cu2+, Zn2+, Ni2+, and Mn2+ cations from mixed aqueous solutions can be prepared by calcination at a suitable temperature and residence time. Regarding the solubility of both the reactive material itself and the precipitates formed, the CCM should contain just a limited content of lime. One way is the calcination of a ferroan magnesite at temperatures above 1000 °C. However, the decrease in pH is accompanied by lower efficiency, attributed to the solid-phase reactions of free lime. A different way is the calcination of magnesite under the conditions when CaCO3 is not thermally decomposed. The virtually complete removal of the heavy metals from the model solution was achieved using the CCM characterised by the fraction of carbonates decomposed of approximately 80% and with the highest specific surface area. CCM calcined at higher temperatures could also be used, but this would be associated with higher consumption of crude magnesite. Under the conditions considered in the present work, the product obtained by the calcination at 750 °C for 3 h appeared to be optimal. The full heavy metal removal was observed in this case using less magnesite, and, moreover, at a lower temperature (resulting, therefore, in a lower consumption of energy for the calcination and material handling).
This study addresses the development of advanced anode materials for lithium-ion batteries by investigating the high-entropy perovskite La(Co0.2Mn0.2Fe0.2Ni0.2Cu0.2)O3. The material was synthesized via spray drying of aqueous metal nitrate solutions, followed by calcination at various temperatures (800 °C/1 h, 1000 °C/1 h, 1000 °C/2 h, 1100 °C/1 h) to optimize structural properties. Structural analysis using X-ray diffraction confirmed the formation of a single-phase perovskite in the sample calcined at 1100 °C for 1 h, while SEM/EDS revealed homogeneous elemental distribution. Electrochemical testing of the powders as anode materials in coin-type lithium-ion cells revealed a trend of slightly increasing capacity over 150 cycles, with capacity ultimately reaching 617 mAh g−1, indicating progressive electrochemical activation. Although the samples share the same composition, variations in calcination conditions resulted in differences in capacity and cycling behavior. These results demonstrate that synthesis parameters critically influence the electrochemical performance of high-entropy perovskites. The findings suggest that such materials have potential as stable anodes for next-generation lithium-ion batteries, contributing to improved durability and efficiency in energy-storage technologies.