Search Results (65)

The present work focuses on the synthesis of a vanadium nitride (VN)/carbon nanocomposite material via the thermal decomposition of vanadyl phthalocyanine (VOPC). The morphology and chemical structure of the synthesized compounds were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), Fourier transformed infrared spectroscopy (FTIR), X-ray diffraction (XRD), and X-ray photoemission spectroscopy (XPS). The successful syntheses of the VOPC and non-metalated phthalocyanine (H₂PC) precursors were confirmed using FTIR and XRD. The VN particles present a needle-like morphology in the VN synthesized by the sol-gel method. The morphology of the VN/C composite material exhibited small clusters of VN particles. The XRD analysis of the thermally decomposed VOPC indicated a mixture of amorphous carbon and VN nanoparticles (VN(TD)) with a cubic structure in the space group FM-3M consistent with that of VN. The XPS results confirmed the presence of V(III)-N bonds in the resultant material, indicating the formation of a VN/C nanocomposite. The VN/C nanocomposite synthesized through thermal decomposition exhibited a high carbon content and a cluster-like distribution of VN particles. The VN/C nanocomposite was used as an anode material in LIBs, which delivered a specific capacity of 307 mAh g⁻¹ after 100 cycles and an excellent Coulombic efficiency of 99.8 at the 100th cycle. Full article

Coupling spectroscopic ellipsometry (SE), quartz crystal microbalance with dissipation (QCM-D), X-ray photoemission spectroscopy (XPS), and atomic force microscopy (AFM), we developed a multi-technique approach to characterize the surface immobilization of probe DNA strands, as a tool for the design of a DNA-based biosensor for the detection of disease-related oligonucleotide strands [...] Full article

Polyethylene terephthalate (PET) microplastics constitute a significant portion of plastic pollution in the environment and pose substantial environmental challenges. In this study, the effectiveness of the Fenton process and post-oxidation coagulation for the removal of non-weathered and UV-weathered PET microplastics (PET MPs) were investigated. A response surface methodology was used to investigate the interplay between PET concentration and ferrous ion (Fe²⁺) concentration. The models revealed an intricate interplay between these variables, highlighting the need for a balanced system for optimal PET MP removal. For non-weathered PET, the simultaneous increase in the concentrations of both PET microplastics and Fe²⁺ was found to enhance the removal efficiency. However, this synergistic effect was not observed in UV-weathered PET, which also demonstrated a more pronounced effect from the Fe²⁺ concentration. The statistical analysis provided a strong basis for the validity of the models. X-ray photoemission spectroscopy (XPS) further elucidated the mechanisms behind these findings, revealing that UV weathering results in surface changes, which facilitate hydroxyl radical oxidation. These findings underline the complexity of the Fenton process in PET microplastic removal and the different behavior of non-weathered and UV-weathered microplastics. This has significant implications for tailoring remediation strategies and underscores the importance of considering environmental weathering in these strategies. Full article

Sputtering of silicon in a He magnetron discharge (MS) has been reported as a bottom-up procedure to obtain He-charged silicon films (i.e., He nanobubbles encapsulated in a silicon matrix). The incorporation of heavier noble gases is demonstrated in this work with a synergistic effect, producing increased Ne and Ar incorporations when using He–Ne and He–Ar gas mixtures in the MS process. Microstructural and chemical characterizations are reported using ion beam analysis (IBA) and scanning and transmission electron microscopies (SEM and TEM). In addition to gas incorporation, He promotes the formation of larger nanobubbles. In the case of Ne, high-resolution X-ray photoelectron and absorption spectroscopies (XPS and XAS) are reported, with remarkable dependence of the Ne 1s photoemission and the Ne K-edge absorption on the nanobubble’s size and composition. The gas (He, Ne and Ar)-charged thin films are proposed as “solid” targets for the characterization of spectroscopic properties of noble gases in a confined state without the need for cryogenics or high-pressure anvils devices. Also, their use as targets for nuclear reaction studies is foreseen. Full article

Currently, electrically conductive polymers based on transition metal complexes [M(Salen)], as well as their composites, are among the systems showing promise as catalysts, electrochromic and electroluminescent materials, and electrodes for energy storage (for batteries and supercapacitors). The current review focuses on elucidating the atomic and electronic structure of metal–salen complexes, their polymers, and composites with nanostructured carbon (carbon nanotubes and graphene) using modern X-ray spectroscopy methods (X-ray photoelectron (XPS) and valence-band photoemission (VB PES) spectroscopy, as well as near-edge (NEXAFS) and extended (EXAFS) X-ray absorption fine structure spectroscopy). We trust that this review will be of valuable assistance to researchers working in the field of synthesizing and characterizing metal–salen complexes and composites based on them. Full article

The exploration initiated by the discovery of the topological insulator (Bi_xSb_1−x)₂Te₃ has extended to unlock the potential of quantum anomalous Hall effects (QAHEs), marking a revolutionary era for topological quantum devices, low-power electronics, and spintronic applications. In this study, we present the epitaxial growth of Cr-doped (Bi_0.4Sb_0.6)₂Te₃ (Cr:BST) thin films via molecular beam epitaxy, incorporating various Cr doping concentrations with varying Cr/Sb ratios (0.025, 0.05, 0.075, and 0.1). High-quality crystalline of the Cr:BST thin films deposited on a c-plane sapphire substrate has been rigorously confirmed through reflection high-energy electron diffraction (RHEED), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM) analyses. The existence of a Cr dopant has been identified with a reduction in the lattice parameter of BST from 30.53 ± 0.05 to 30.06 ± 0.04 Å confirmed by X-ray diffraction, and the valence state of Cr verified by X-ray photoemission (XPS) at binding energies of ~573.1 and ~583.5 eV. Additionally, the influence of Cr doping on lattice vibration was qualitatively examined by Raman spectroscopy, revealing a blue shift in peaks with increased Cr concentration. Surface characteristics, crucial for the functionality of topological insulators, were explored via Atomic Force Microscopy (AFM), illustrating a sevenfold reduction in surface roughness as the Cr concentration increased from 0 to 0.1. The ferromagnetic properties of Cr:BST were examined by a superconducting quantum interference device (SQUID) with a magnetic field applied in out-of-plane and in-plane directions. The Cr:BST samples exhibited a Curie temperature (T_c) above 50 K, accompanied by increased magnetization and coercivity with increasing Cr doping levels. The introduction of the Cr dopant induces a transition from n-type ((Bi_0.4Sb_0.6)₂Te₃) to p-type (Cr:(Bi_0.4Sb_0.6)₂Te₃) carriers, demonstrating a remarkable suppression of carrier density up to one order of magnitude, concurrently enhancing carrier mobility up to a factor of 5. This pivotal outcome is poised to significantly influence the development of QAHE studies and spintronic applications. Full article

This paper investigates the bipolar resistive switching and synaptic characteristics of IZO single-layer and IZO/SiO₂ bilayer two-terminal memory devices. The chemical properties and structure of the device with a SiO₂ layer are confirmed by x-ray photoemission spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The device with the SiO₂ layer showed better memory characteristics with a low current level, as well as better cell-to-cell and cycle-to-cycle uniformity. Moreover, the neuromorphic applications of the IZO/SiO₂ bilayer device are demonstrated by pulse response. Paired pulse facilitation, excitatory postsynaptic current, and pulse-width-dependent conductance changes are conducted by the coexistence of short- and long-term memory characteristics. Moreover, Hebbian rules are emulated to mimic biological synapse function. The result of potentiation, depression, spike-rate-dependent plasticity, and spike-time-dependent plasticity prove their favorable abilities for future applications in neuromorphic computing architecture. Full article

Metal–organic chemical vapor deposition (MOCVD) is a key method for scalable synthesis of two-dimensional transition metal dichalcogenide (2D-TMDC) layers. However, it faces several challenges, such as the unintentional co-deposition of carbon impurities resulting from the pyrolysis of metal–organic precursors. This study investigates the chemical features of carbon and its impact on the photoluminescence property and air stability of 2D-MoS₂. Using X-ray photoemission spectroscopy (XPS), it was found that the carbon impurities show characteristics similar to those of sp²-bonded graphitic carbon. Upon prolonged (20–40 weeks) exposure to the atmosphere, the incorporated carbon appears to react with 2D-MoS_2, forming a MoS_2−xC_x solid solution. At the same time, a gradual decrease in the S/Mo ratio implies the formation of sulfur vacancies was also observed. These two processes lead to crystal degradation over time, as evidenced by the gradual quenching of the Raman and photoluminescence (PL) peaks. More detailed PL analyses suggest a charge transfer mechanism between sp²-carbon/2D-MoS₂ and 2D-MoS₂/air-adsorbates, which, in the short term, could alter PL emissions and appear to further intensify the degradation of 2D-MoS₂ in the long-term. The findings highlight the strong impact of unintentionally co-deposited carbon on the optical properties and air stability of MOCVD 2D-MoS₂ layers. Full article

Here, a novel copper p-aminophenol metal–organic framework (Cu(PAP)₂) is first reported. Powder X-ray diffraction (PXRD), infrared spectra (FTIR), Raman spectra, transmission electron microscopy (TEM) and X-ray photoemission spectroscopy (XPS), in combination with a structure simulation, indicated that Cu(PAP)₂ is a two-dimensional (2D) material with a staggered structure analogous to that of graphite. Based on its 2D graphite-like layer structure, Cu(PAP)₂ was expected to exhibit preferable tribological behaviors as an additive in liquid lubricants, and the tribological properties of Cu(PAP)₂ as a lubricating additive in hydrogenated polydecene (PAO6) or deionized water were investigated. Compared to PAO6 or deionized water, the results indicated that deionized water-based Cu(PAP)₂ showed much better friction reduction and anti-wear behavior than PAO6-based Cu(PAP)₂ did, which was due to Cu(PAP)₂ penetrating the interface between friction pairs in deionized water, but not in PAO6, thus producing lower friction and wear resistance values. Full article

Preparing protecting coatings on the surface of Zr claddings has been regarded as one of the accident tolerant fuel (ATF) strategies. In this study, a series of nitride-modified layers were in situ grown by hollow cathode plasma nitriding on the surface of Zr metal. The influence of nitriding currents and time on the phases, composition, microstructure and corrosion resistance of the modified layers was investigated by X-ray diffraction (XRD), X-ray Photoemission Spectroscopy (XPS), transmission electron microscope (TEM), scanning electron microscopy (SEM) with energy dispersive spectrometer (EDS) and potentiodynamic polarization curves. The ZrO₂ layer with loose microstructure and cracks prefers to form under low nitriding current of 0.4 A, which also causes poor corrosion resistance. The high temperature caused by high nitriding currents (0.6 A and 0.8 A) promote the formation of compact nanocrystalline layers, made up of nitride and oxynitride. Below the nanocrystalline layer, it is Zr₂N caused by N penetration. Besides this, a double-layer structure of the nanocrystalline layer, i.e., an equiaxed crystal zone with a grain size of ~10–50 nm on the surface and a long strip grain region beneath it was observed. The compact nitride/oxynitride layer with excellent interface bonding can improve the corrosion resistance effectively. Full article

A comparative study of the electronic structure of the salen ligand in the H₂(Salen) molecule and the [Ni(Salen)] complex was performed using the experimental methods of XPS, UV PES, and NEXAFS spectroscopy along with DFT calculations. Significant chemical shifts of +1.0 eV (carbon), +1.9 eV (nitrogen), and −0.4 eV (oxygen) were observed in the 1s PE spectra of the salen ligand atoms when passing from a molecule to a complex, unambiguously indicating a substantial redistribution of the valence electron density between these atoms. It is proposed that the electron density transfer to the O atoms in [Ni(Salen)] occurred not only from the Ni atom, but also from the N and C atoms. This process seemed to be realized through the delocalized conjugated π-system of the phenol C 2p electronic states of the ligand molecule. The DFT calculations (total and partial DOS) for the valence band H₂(Salen) and [Ni(Salen)] described well the spectral shape of the UV PE spectra of both compounds and confirmed their experimental identification. An analysis of the N and O 1s NEXAFS spectra clearly indicated that the atomic structure of the ethylenediamine and phenol fragments was retained upon passing from the free salen ligand to the nickel complex. Full article

This paper reports on improved AlGaN/GaN metal oxide semiconductor high-electron mobility transistors (MOS-HEMTs). TiO₂ is used to form the dielectric and passivation layers. The TiO₂ film is characterized using X-ray photoemission spectroscopy (XPS), Raman spectroscopy, and transmission electron microscopy (TEM). The quality of the gate oxide is improved by annealing at 300 °C in N₂. Experimental results indicate that the annealed MOS structure effectively reduces the gate leakage current. The high performance of the annealed MOS-HEMTs and their stable operation at elevated temperatures up to 450 K is demonstrated. Furthermore, annealing improves their output power characteristics. Full article

Here, I fill large 1.7 nm diameter single-walled carbon nanotubes (SWCNTs) with silver chloride (AgCl). I present photoemission insights into the filling of SWCNTs. C1s X-ray photoelectron spectroscopy (XPS) reveals the p-doping of SWCNTs. The Raman spectroscopy data are complementary to the XPS data, and they confirm the strong doping effect of encapsulated silver chloride on SWCNTs. Full article

The role of minerals in the origin of life and prebiotic evolution remains unknown and controversial. Mineral surfaces have the potential to facilitate prebiotic polymerization due to their ability to adsorb and concentrate biomolecules that subsequently can catalyse reactions; however, the precise nature of the interaction between the mineral host and the guest biomolecule still needs to be understood. In this context, we spectroscopically characterized, using infrared, X-ray photoemission spectroscopy (XPS) and X-ray diffraction (XRD) techniques, the interaction between L-proline and montmorillonite, olivine, iron disulphide, and haematite (minerals of prebiotic interest), by evaluating their interaction from a liquid medium. This work provides insight into the chemical processes occurring between proline, the only cyclic amino acid, and this selection of minerals, each of them bearing a particular chemical and crystal structures. Proline was successfully adsorbed on montmorillonite, haematite, olivine, and iron disulphide in anionic and zwitterionic chemical forms, being the predominant form directly related to the mineral structure and composition. Silicates (montmorillonite) dominate adsorption, whereas iron oxides (haematite) show the lowest molecular affinity. This approach will help to understand structure-affinity relationship between the mineral surfaces and proline, one of the nine amino acids generated in the Miller-Urey experiment. Full article

The surface properties of drug containers should reduce the adsorption of the drug and avoid packaging surface/drug interactions, especially in the case of biologically-derived products. Here, we developed a multi-technique approach that combined Differential Scanning Calorimetry (DSC), Atomic Force Microscopy (AFM), Contact Angle (CA), Quartz Crystal Microbalance with Dissipation monitoring (QCM-D), and X-ray Photoemission Spectroscopy (XPS) to investigate the interactions of rhNGF on different pharma grade polymeric materials. Polypropylene (PP)/polyethylene (PE) copolymers and PP homopolymers, both as spin-coated films and injected molded samples, were evaluated for their degree of crystallinity and adsorption of protein. Our analyses showed that copolymers are characterized by a lower degree of crystallinity and lower roughness compared to PP homopolymers. In line with this, PP/PE copolymers also show higher contact angle values, indicating a lower surface wettability for the rhNGF solution on copolymers than PP homopolymers. Thus, we demonstrated that the chemical composition of the polymeric material and, in turn, its surface roughness determine the interaction with the protein and identified that copolymers may offer an advantage in terms of protein interaction/adsorption. The combined QCM-D and XPS data indicated that protein adsorption is a self-limiting process that passivates the surface after the deposition of roughly one molecular layer, preventing any further protein adsorption in the long term. Full article