Herein we report on an environmentally friendly and scalable production route for hollow silica spheres (HSSs). The process is based on close to 100% conversion of non-crystalline solid Si nanoparticles ( = 40 ± 9 nm) in mild alkaline solutions (pH ≤ 9.0) at ambient temperature. The Si nanoparticles are prepared using the centrifugal chemical vapor deposition (cCVD) method. Combining transmission electron microscopy (TEM) imaging and nanoparticle size analysis with hydrogen evolution data, elemental mapping, and nitrogen adsorption for surface area measurement, we show for the first time experimental data that document a Kirkendall type Si-to-HSS formation process. Our understanding is that the Si nanoparticles exposed to air form a SiO₂ film, which is stable in the mild alkaline environment. Silicon from the Si nanoparticles is transported through the thin SiO₂ film and is reacting with H₂O/OH⁻ species on the particle surface or in the already thickened SiO₂ shell to form silicic acid that in turn rapidly gets converted to a sol–gel to continue the growing of the silica shell. We foresee that this green chemistry approach can be utilized for HSS preparation for use in batteries, insulation materials and drug delivery.

Tetrataenite is a promising candidate for rare earth-free permanent magnets due to its low cost and intrinsic magnetic properties. This work investigates the effect of combined milling at liquid nitrogen temperatures (cryomilling) and the addition of carbon as an interstitial element for promoting the formation of tetrataenite. Crystal structure, microstructure, and magnetic properties are investigated to understand the influence of mechanical processing and compositional modifications. No unambiguous evidence of the ordered phase of tetrataenite is found in the structural characterization. However, using Scanning Transmission Electron Microscopy (STEM) and powder X-ray diffraction (PXD) analyses, the occurrence of both twinning and stacking faults resulting from the high-energy milling process is observed, which is a relevant factor for identifying tetrataenite in FeNi alloys. The probability of a stacking fault and twinning occurring for a carbon-free FeNi sample before annealing is found to be 2% and 1.4%, respectively. After annealing, the stacking fault probability decreased to 1.2%, while that of twinning was 1.4%. By increasing the carbon concentration to 5 at.%, the stacking faults and twinning probabilities decrease slightly to 1.2% and 1.3%, respectively. The occurrence of stacking faults combined with small crystallite sizes was a hindering factor in identifying the presence of tetrataenite.