This article presents the results of the formation of hierarchical micro–nano structures in nanostructured tin dioxide films obtained from the lyophilic film-forming system SnCl4/EtOH/NH4OH. The classification of the shape and size of the synthesized structures, in relation to the pH of the solution, is presented. Measurements were carried out on an X-ray diffractometer to study the crystal structure of the samples analyzed. It was found that SnO2 and NH4Cl crystallites participate in the formation of the synthesized hierarchical structures. It is shown that the mechanism of the formation of hierarchical structures depends on the amount of ammonium hydroxide added. This makes it possible to control the shape and size of the synthesized structures by changing the ratio of precursors.
In this paper, we investigated fractal cluster structures of colloidal particles in tin dioxide films obtained from lyophilic film-forming systems SnCl4/EtOH/NH4OH with different pH levels. It was revealed that at the ratio Sn > Cl2 > O2, N2 = 0, and pH = 1.42, the growth of cross-shaped and flower-shaped structures of various sizes from several μm to tens of μm is observed. At the ratio Cl2 > Sn > O2 > N2 and pH = 1.44, triangular and hexagonal structures are observed, the sizes of which are on the order of several tens of micrometers. The growth of hexagonal structures is probably affected by the presence of nitrogen in the film, according to the elemental analysis data. At the ratio Sn > Cl2 > O2 > N2 and solution pH of 1.49, the growth of hexagonal and cross-shaped structures is observed, whereas flower-shaped structures are not observed. Hierarchical flower-like and cross-shaped structures are fractal. The shape of microstructures is directly related to the shape of the elementary cells of SnO2 and NH4Cl. A direct dependence of the formation of hierarchical structures on the volume of ammonium hydroxide additive was found. This allows for controlling the shape and size of the synthesized structures when changing the ratio of the initial precursors and influencing the final physicochemical characteristics of the obtained samples.
Lithium-ion battery (LIB) recycling is usually compared across pyrometallurgical, hydrometallurgical and direct routes as if the optimal route were independent of the cathode being recycled. This review argues that cathode chemistry is the governing variable. Following the chain from cathode chemistry and degradation mechanism through pretreatment, recycling route and recovered product to electrochemical validation, we compare LiNixMnyCozO2 (NMC, 111 to 811) and LiFePO4 (LFP), with LiCoO2 and LiNi0.8Co0.15Al0.05O2 as references. LFP degradation is dominated by Li loss and Fe/Li anti-site defects in an intact olivine framework, which makes direct regeneration mechanistically well founded. Ni-rich NMC suffers microcracking, surface reconstruction and proton sensitivity, so its regeneration increasingly becomes upcycling into a different product, whereas hydrometallurgical resynthesis currently has the strongest industrial validation. Reported recovery efficiencies above 95% rarely demonstrate battery-grade products, and published energy estimates for the same route and chemistry differ by a factor of up to about 1.5 because of inconsistent system boundaries. We propose a cathode-to-cathode circularity framework and a minimum reporting set that link material recovery to validation in new cells.