Seeded Growth of Type-II Na24Si136 Clathrate Single Crystals

Type-II Na24Si136 clathrate octahedral single crystals surrounded by {111} facets were grown by evaporating Na from a molten mixture of Na4Si4 and Na9Sn4 at 823 K for 12 h. One of the obtained single crystals was used as a seed for the following single crystal growth of the type-II clathrate using the same method. The single crystal grown on the seed maintained the octahedral shape. The weight of the crystal grown with the seed was increased from 0.6 to 30.4 mg by repeating the seeded growth and was proportional to the surface area of the seed crystal.

Deposition of Arsenic from Nitric Acid Leaching Solutions of Gold–Arsenic Sulphide Concentrates

At present, the processing of refractory gold–arsenic sulphide concentrates is becoming more relevant due to the depletion of rich crude ore reserves. In the process of the nitric acid leaching of arsenic sulphide minerals, solutions are formed containing 20–30 g/L of arsenic (III). Since market demand for arsenic compounds is limited, such solutions are traditionally converted into poorly soluble compounds. This paper describes the investigation of precipitating arsenic sulphide from nitric acid leaching solutions of refractory sulphide raw materials of nonferrous metals containing iron (III) ions using sodium hydrosulphide with a molar ratio of NaHS/As = 2.4–2.6, which is typical for pure model solutions without oxidants. The work studied the effect of temperature, the pH of the solution and the consumption of NaHS and seed crystal on this process. The highest degree of precipitation of arsenic (III) sulphide (95–99%) from nitric acid leaching solutions containing iron (III) ions without seed occurs with a pH from 1.8 to 2.0 and a NaHS/As molar ratio of 2.8. The introduction of seed crystal significantly improves the precipitation of arsenic (III) sulphide. An increase in seed crystal consumption from 0 to 34 g/L in solution promotes an increase in the degree of transition of arsenic to sediment from 36.2 to 98.1% at pH = 1. According to SEM/EDS and XRF sediment data, from the results of experiments on the effect of As2S3 seed crystal consumption, acidity and molar ratio of NaHS/As on the precipitation of arsenic (III) sulphide and the Fetotal/Fe2+ ratio in the final solution, it can be concluded that the addition of a seed accelerates the crystallisation of arsenic (III) sulphide by increasing the number of crystallisation centres; as a result, the deposition rate of As2S3 becomes higher. Since the oxidation rate of sulphide ions to elemental sulphur by iron (III) ions does not change significantly, the molar ratio of NaHS/As can be reduced to 2.25 to obtain a precipitate having a lower amount of elemental sulphur and a high arsenic content similar to that precipitated from pure model solutions.

Phosphorus Recovery From Waste Activated Sludge by Sponge Iron Seeded Crystallization of Vivianite and Process Optimization With Response Surface Methodology

As a novel phosphorus recovery product, vivianite (Fe3(PO4)2·8H2O) has attracted much attention due to its enormous recycling potential and foreseeable economic value. Taking sponge iron as seed material, the effect of different reaction conditions on the recovery of phosphorus in waste activated sludge by vivianite crystallization was studied. Through single factor test, the optimal conditions for vivianite formation were in the pH range of 5.5–6.0 with Fe/P molar ratio of 1.5. Scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and energy dispersive spectroscopy (EDS) were used to analyze the components of the crystals. The results showed that the vivianite produced with sponge iron as the seed crystal were larger and thicker (300-700 μm) than other seed (200-300 μm) and without seed (50-100 μm). Moreover, vivianite, which was synthesized with sponge iron as seed, was obviously magnetic and could be separated from sludge by rubidium magnet. The Box-Behnken design of the response surface methodology was used to optimize the phosphorus-recovery process with sponge iron (maximum phosphorus recovery rate was 83.17%), and the interaction effect of parameters was also examined. PH had a significant effect on the formation of vivianite. In summary, this research verifies the feasibility of using sponge iron as seed crystal to recover phosphorus in the form of vivianite from waste activated sludge, which is conducive to the subsequent separation and utilization of vivianite.

Al-ZSM-5 Nanocrystal Catalysts Grown from Silicalite-1 Seeds for Methane Conversion

This study evaluated Al-ZSM-5 nanocrystals grown from silicalite-1 seed crystals as catalysts for the methane dehydroaromatization (MDA) reaction. Silicalite-1 seed crystals sized between 30 and 40 nm were used to grow Al-ZSM-5 under various synthesis conditions. The size of Al-ZSM-5 was significantly affected by the Si/Al ratio (SAR), synthesis time, and silica nutrients/seed crystal ratio (NSR). Larger crystals were obtained with an increased SAR in the synthesis sols. Gradual growth of Al-ZSM-5 occurred with synthesis time, although the growth in crystal size ceased at 5 h of synthesis at 120 °C, indicating the rapid growth of Al-ZSM-5 aided by the silicalite-1 seeds. Precise tuning of Al-ZSM-5 size was possible by changing the nutrient/silicalite-1 seed ratio; a higher NSR led to larger crystals. Two representative Al-ZSM-5 crystals with SARs of 35 and 140 were prepared for catalyst testing, and the crystal sizes were tailored to <100 nm by controlling NSR. The MDA reaction was conducted in the presence of the prepared Al-ZSM-5. The catalyst size exhibited distinct differences in catalyst stability, while the SAR of catalysts did not produce noticeable changes in the catalyst stability of the Al-ZSM-5 crystals and commercial zeolites in this reaction system.

Seed crystal free growth of high-quality double cation – double halide perovskite single crystals for optoelectronic applications

We developed a seed crystal free re-fill crystallization method (RFCM) to grow high-quality (FAPbI3)0.9(MAPbBr3)0.1 perovskite single crystals for optoelectronic applications.