Magnetron sputter inert gas condensation was coupled with quadrupole mass spectrometry for the in situ characterization of a nanoparticle beam. The proposed method allows us to determine the size distribution and the mass flux of the nanoparticles. The measured quadrupole mass spectrometer grid current is converted into a nanoparticle flux and subsequently into a mass flux. Cu nanoparticles were deposited onto Si substrates using different filtering modes of the quadrupole mass spectrometer. Characterization was carried out using a combination of x-ray photoelectron spectroscopy and scanning electron microscopy. Quantitative analysis of the elemental composition of the Si surface revealed a Gaussian distribution of the deposited nanoparticles over the diameter of the rotating substrate holder with a good quantitative agreement with the predictions made from the in situ quantification method.

In recent nanomaterials research, combining nanoporous carbons with metallic nanoparticles, like palladium (Pd), has emerged as a focus due to their potential in energy, environmental and biomedical fields. This study presents a novel approach for synthesizing Pd-decorated carbons using magnetron sputter deposition. This method allows for the functionalization of nanoporous carbon surfaces with Pd nano-sized islands, creating metal–carbon nanocomposites through brief deposition times of up to 15 s. The present research utilized direct current magnetron sputtering to deposit Pd islands on a flexible activated carbon cloth substrate. The surface chemistry, microstructure, morphology and pore structure were analyzed using a variety of material characterization techniques, including X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectroscopy, gas sorption analysis and scanning electron microscopy. The results showed Pd islands of varying sizes distributed across the cloth’s carbon fibers, achieving high-purity surface modifications without the use of chemicals. The synthesis method preserves the nanoporous structure of the carbon cloth substrate while adding functional Pd islands, which could be potentially useful in emerging fields like hydrogen storage, fuel cells and biosensors. This approach demonstrates the possibility of creating high-quality metal–carbon composites using a simple, clean and economical method, expanding the possibilities for future nanomaterial-based applications.

Nanoparticles are essential for energy storage, catalysis, and medical applications, emphasizing their accurate chemical characterization. However, atom probe tomography (APT) of nanoparticles sandwiched at the interface between an encapsulating film and a substrate poses difficulties. Poor adhesion at the film-substrate interface can cause specimen fracture during APT, while impurities may introduce additional peaks in the mass spectra. We demonstrate preparing APT specimens with strong adhesion between nanoparticles and film/substrate matrices for successful analysis. Copper nanoparticles were encapsulated at the interface between nickel film and cobalt substrate using electrodeposition. Cobalt and nickel were chosen to match their evaporation fields with copper, minimizing peak overlaps and aiding nanoparticle localization. Copper nanoparticles were deposited via magnetron sputter inert gas condensation with varying deposition times to yield suitable surface coverages, followed by encapsulation with the nickel film. In-plane and cross-plane APT specimens were prepared by femtosecond laser ablation and focused ion beam milling. Longer deposition times resulted in agglomerated nanoparticles as well as pores and voids, causing poor adhesion and specimen failure. In contrast, shorter deposition times provided sufficient surface coverage, ensuring strong adhesion and reducing void formation. This study emphasizes controlled surface coverage for reliable APT analysis, offering insights into nanoparticle chemistry.

Metal–carbon nanocomposites are identified as key contenders for enhancing water splitting through the oxygen evolution reaction and boosting supercapacitor energy storage capacitances. This study utilizes plasma treatment to transform natural graphite into nanoporous few-layer graphene, followed by additional milling and plasma steps to synthesize a cobalt–graphene nanocomposite. Comprehensive structural characterization was conducted using scanning and transmission electron microscopy, X-ray diffraction, Raman spectroscopy, gas sorption analysis and X-ray photoelectron spectroscopy. Electrochemical evaluations further assessed the materials’ oxygen evolution reaction and supercapacitor performance. Although the specific surface area of the nanoporous carbon decreases from 780 to 480 m²/g in the transition to the resulting nanocomposite, it maintains its nanoporous structure and delivers a competitive electrochemical performance, as evidenced by an overpotential of 290 mV and a Tafel slope of 110 mV/dec. This demonstrates the efficacy of plasma treatment in the surface functionalization of carbon-based materials, highlighting its potential for large-scale chemical-free application due to its environmental friendliness and scalability, paving the way toward future applications.