Commercial micrometer silicon (Si) powder was investigated as a potential anode material for lithium ion (Li-ion) batteries. The characterization of this powder showed the mean particle size of approx.75.2 nm, BET surface area of 10.6 m^2/g and average pore size of 0.56 nm. Its band gap was estimated to 1.35 eV as determined using UV-Vis diffuse reflectance spectra. In order to increase the surface area and porosity which is important for Li-ion batteries, the starting Si powder was ball-milled and threatened by metal-assisted chemical etching. The mechanochemical treatment resulted in decrease of the particle size from 75 nm to 29 nm, an increase of the BET surface area and average pore size to 16.7 m²/g and 1.26 nm, respectively, and broadening of the X-ray powder diffraction (XRD) lines. The XRD patterns of silver metal-assisted chemical etching (MACE) sample showed strong and narrow diffraction lines typical for powder silicon and low-intensity diffraction lines typical for silver. The metal-assisted chemical etching of starting Si material resulted in a decrease of surface area to 7.3 m²/g and an increase of the average pore size to 3.44 nm. These three materials were used as the anode material in lithium-ion cells, and their electrochemical properties were investigated by cyclic voltammetry and galvanostatic charge-discharge cycles. The enhanced electrochemical performance of the sample prepared by MACE is attributed to increase in pore size, which are large enough for easy lithiation. These are the positive aspects of the application of MACE in the development of an anode material for Li-ion batteries.

Magnetic polymer gels are a new promising class of nanocomposite gels. In this work, magnetic PEO/iron oxide nanocomposite hydrogels were synthesized using the one-step γ-irradiation method starting from poly(ethylene oxide) (PEO) and iron(III) precursor alkaline aqueous suspensions followed by simultaneous crosslinking of PEO chains and reduction of Fe(III) precursor. γ-irradiation dose and concentrations of Fe³⁺, 2-propanol and PEO in the initial suspensions were varied and optimized. With 2-propanol and at high doses magnetic gels with embedded magnetite nanoparticles were obtained, as confirmed by XRD, SEM and Mössbauer spectrometry. The quantitative determination of γ-irradiation generated Fe²⁺ was performed using the 1,10-phenanthroline method. The maximal Fe²⁺ molar fraction of 0.55 was achieved at 300 kGy, pH = 12 and initial 5% of Fe³⁺. The DSC and rheological measurements confirmed the formation of a well-structured network. The thermal and rheological properties of gels depended on the dose, PEO concentration and initial Fe³⁺ content (amount of nanoparticles synthesized inside gels). More amorphous and stronger gels were formed at higher dose and higher nanoparticle content. The properties of synthesized gels were determined by the presence of magnetic iron oxide nanoparticles, which acted as reinforcing agents and additional crosslinkers of PEO chains thus facilitating the one-step gel formation.

In this study, we present a new approach for the synthesis of Pt/SnO₂ catalysts using microwave radiation. Pt(IV) and Sn(IV) inorganic precursors (H₂PtCl₆ and SnCl₄) and ammonia were used, which allowed the controlled formation of platinum particles on the anisotropic SnO₂ support. The synthesized Pt/SnO₂ samples are mesoporous and exhibit a reversible physisorption isotherm of type IV. The XRD patterns confirmed the presence of platinum maxima in all Pt/SnO₂ samples. The Williamson-Hall diagram showed SnO₂ anisotropy with crystallite sizes of ~10 nm along the c-axis (< 00l >) and ~5 nm along the a-axis (< h00 >). SEM analysis revealed anisotropic, urchin-like SnO₂ particles. XPS results indicated relatively low average oxidation states of platinum, close to Pt metal. ¹¹⁹Sn Mössbauer spectroscopy indicated electronic interactions between Pt and SnO₂ particles. The synthesized samples were used for the catalytic reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the presence of excess NaBH₄. The catalytic activity of the Pt/SnO₂ samples for the reduction of 4-NP to 4-AP was optimized by varying the synthesis parameters and Pt loading. The optimal platinum loading for the reduction of 4-NP to 4-AP on the anisotropic SnO₂ support is 5 mol% with an apparent rate constant k = 0.59 × 10^–2 s^–1. The Pt/SnO₂ sample showed exceptional reusability and retained an efficiency of 81.4% after ten cycles.

The dispersion of platinum (Pt) on metal oxide supports is important for catalytic and gas sensing applications. In this work, we used mechanochemical dispersion and compatible Fe(II) acetate, Sn(II) acetate and Pt(II) acetylacetonate powders to better disperse Pt in Fe₂O₃ and SnO₂. The dispersion of platinum in SnO₂ is significantly different from the dispersion of Pt over Fe₂O₃. Electron microscopy has shown that the elements Sn, O and Pt are homogeneously dispersed in α-SnO₂ (cassiterite), indicating the formation of a (Pt,Sn)O₂ solid solution. In contrast, platinum is dispersed in α-Fe₂O₃ (hematite) mainly in the form of isolated Pt nanoparticles despite the oxidative conditions during annealing. The size of the dispersed Pt nanoparticles over α-Fe₂O₃ can be controlled by changing the experimental conditions and is set to 2.2, 1.2 and 0.8 nm. The rather different Pt dispersion in α-SnO₂ and α-Fe₂O₃ is due to the fact that Pt⁴⁺ can be stabilized in the α-SnO₂ structure by replacing Sn⁴⁺ with Pt⁴⁺ in the crystal lattice, while the substitution of Fe³⁺ with Pt⁴⁺ is unfavorable and Pt⁴⁺ is mainly expelled from the lattice at the surface of α-Fe₂O₃ to form isolated platinum nanoparticles.

An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO₂ supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO₂ supports, namely SnA (synthesized almost at room temperature), SnB (hydrothermally treated at 180 °C), and SnC (annealed at 600 °C), are systematically investigated, all loaded with 1 mol% Pt from H₂PtCl₆ under identical mild conditions. The chloride ions from the SnCl₄ precursors were efficiently removed via a strong-base anion exchange reaction, resulting in highly dispersed, crystalline ~5 nm cassiterite SnO₂ particles. All Pt/SnO₂ composites displayed mesoporous structures with type IVa isotherms and H₂-type hysteresis, with SP1a (Pt on SnA) exhibiting the largest surface area (122.6 m²/g) and the smallest pores (~3.5 nm). STEM-HAADF imaging revealed well-dispersed PtOx domains (~0.85 nm), while XPS confirmed the dominant Pt⁴⁺ and Pt²⁺ species, with ~25% Pt⁰ likely resulting from photoreduction and/or interactions with Sn–OH surface groups. Raman spectroscopy revealed three new bands (260–360 cm⁻¹) that were clearly visible in the sample with 10 mol% Pt and were due to the vibrational modes of the PtOx species and Pt-Cl bonds introduced due the addition and hydrolysis of H₂PtCl₆ precursor. TGA/DSC analysis revealed the highest mass loss for SP1a (~7.3%), confirming the strong hydration of the PtOx domains. Despite the predominance of oxidized PtOx species, SP1a exhibited the highest catalytic activity (k_app = 1.27 × 10⁻² s⁻¹) and retained 84.5% activity for the reduction of 4-NP to 4-AP after 10 cycles. This chloride-free low-temperature synthesis route offers a promising and generalizable strategy for the preparation of noble metal-based nanocatalysts on oxide supports with high catalytic activity and reusability.