ZnFe 2 O 4 ferrite nanoparticles are arousing a great interest in the biomedical field, thanks to their superparamagnetic behavior at room temperature. Functional properties depend on composition, size, nanoparticle architecture and, in turn, on the synthesis methods. Bulk ZnFe 2 O 4 has the normal spinel structure (all Zn 2+ ions in tetrahedral and all Fe 3+ ions in octahedral positions), but at the nanometric size inversion takes place with a cationic mixing on divalent and trivalent sites. The sensitivity of the Raman probe to cation disorder favored the appearance of several works on a rich variety of nanosized zinc ferrites. An overview on these results is reported and discussed at variance with synthesis methods, grain dimensions, and dopants. We add to this landscape our results from new nanosized powder samples made by microwave-assisted combustion, with different dopants (Ca, Sr on Zn site and Al, Gd on Fe site). A detailed analysis of A 1g , E g , 3F 2g Raman modes has been performed and Raman band parameters have been derived from bestfitting procedures and carefully compared to literature data. The vibrational results are discussed taking into account the characterization from X-ray powder diffraction raction, SEM-EDS probe, EPR spectroscopy and, of course, the magnetic responses.
Black phosphorus (BP) is a two-dimensional material potentially of great interest for applications in the fields of energy, sensing, and microelectronics. One of the most interesting methods to obtain BP is the conversion from red phosphorus (RP) by means of high-energy mechanochemical synthesis. To date, however, this synthesis process was not well characterized. In this work, starting from the mathematical model of energy transfer during the ball milling process, we investigate the effects on RP → BP conversion of three experimental parameters, the rotation speed, the milling time, and the weight ratio between the spheres and the milled material (BtPw ratio). The efficiency of the conversion process was verified by solid-state NMR, Raman spectroscopy, and X-ray diffraction. Whereas the first two parameters have a minor importance, the BtPw ratio plays a primary role in the RP → BP conversion. Yields approaching 100% can be obtained also with short milling times (15 min) and adequate rotation speed (e.g., 500 r.p.m.), provided that the BtPw ratio >40:1 is used. These results confirm the energy sustainability of the mechanochemical synthesis approach.
The adhesion and proliferation of bacteria on abiotic surfaces pose challenges in both health care and industrial applications. Gold nanostars (GNSs) monolayers grafted on glass have demonstrated to exert antibacterial action due to their photo-thermal features. Here, these GNS layers were further functionalized using thiols monolayers, in order to impart different wettability to the surfaces and thus adding a feature that could help to fight bacterial proliferation. Thiol that has different functional groups was used and the thiol-protected surfaces were characterized by means of UV-vis spectroscopy, contact angles, SEM and surface enhanced Raman spectroscopy (SERS). We verified that (i) coating with the proper thiol allows us to impart high hydrophilicity or hydrophobicity to the surfaces (with contact angle values ranging from 10 to 120°); (ii) GNS monolayers are strongly stabilized by functionalization with thiols, with shelf stability increasing from a few weeks to more than three months and (iii) photo-thermal features and subsequent antibacterial effects caused by hyperthermia are not changed by thiols layers, allowing us to kill at least 99.99% of representative bacterial strains.
In the present work, we show a successful approach to achieve stable structural and optical changes induced by pressure on bulk amounts of MAPI after pressure release.
We prepared and characterized recyclable surface enhanced Raman spectroscopy (SERS) active glass chips. Gold nanostars were grafted on properly functionalized glasses by means of electrostatic interactions and then they were coated with a silica layer of controllable thickness in the nanometer range. The SERS activity of the obtained substrates were tested in terms of reproducibility and homogeneity intra-samples and inter-samples from different batches using the Raman reporter as the model compound rhodamine 6G. The uncoated substrates were used as reference to evaluate the effect of silica spacers on SERS enhancement factors (EFs). The chemical route to obtain silica-coated SERS chips is described in detail, and the morphology and the optical response of substrates have been characterized. We demonstrate that SERS substrates coated with 1 nm silica conserve a good EF, and that the coating confers to the SERS platform an extreme robustness leading to reusability of the substrates.
The search for highly performing cathode materials for sodium batteries is a fascinating topic. Unfortunately, Na0.44MnO2 (NMO), the well-known cathode material with good electrochemical performances, suffers from structural degradation due to reduction of Mn4+ to the Jahn–Teller Mn3+ ion, limiting the long-term cyclability. The cation substitution can be a useful way to mitigate the problem, thanks to the possible stabilization of mixtures of different polymorphs. In this paper, NMO was first substituted with Fe ions, obtaining Na0.44Mn0.5Fe0.5O2, with layered structure, then Al, Si and Cu (10% atom) were substituted on both Mn and Fe ions. Mixtures of P3 type phases, in different amount depending on dopant, were obtained and quantified by Rietveld refinements, and relationships between chemical composition, polymorph type and morphology were proposed. Cyclic voltammetry showed broad peaks, due to the complex structural transitions consequent to the intercalation/deintercalation of sodium. Charge discharge cycles disclosed the superior performances of Cu doped sample, which also benefits from improved air stability, a well-known issue of layered compounds. Discharge capacity values of about 63 mAh/g were detected at 1C, and after 50 cycles at C/2, capacities of about 80 mAh/g are obtained, with a capacity retention of 86%.
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