In this paper we accurately revisit the mechanical exfoliation and layer number determination of MoS ₂ . By modelling the exfoliation itself as a random vertical (lateral) exfoliation (fragmentation) phenomenon, a rationale is given to optimise the number of iterations in the scotch-tape peeling technique and we rigorously demonstrate that since the second cleavage the occurrence of monolayers is the most likely. For the unambiguous layer number identification, experiments have been carried out with a unified complementary approach based on optical microscopy, atomic force microscopy, resonant and non resonant Raman spectroscopy, and photo-luminescence spectroscopy. The experimental analysis has been carried out on a statistically significant set of few-layer MoS ₂ flakes (from one to five layers). The work stresses the strong need of such complementary multi-technique approach to really unambiguously determine the layer number of flakes (that neither optical microscopy, nor AFM alone can give). Optical microscopy contrast analysis experiments (carried out on flakes deposited onto 270 nm SiO ₂ /Si(1 0 0) substrates) demonstrate that for few-layer MoS ₂ (from the mono to the epta-layer) the optical contrast is weakly depending on the radiation wavelength and is a non-monotonic function of the layer number. Thus, flakes from ten to twelve layers exhibit the same contrast of monolayers, as demonstrated by parallel AFM analysis. AFM clearly shows that the stacking between the silicon oxide substrate and the first MoS ₂ layer is strongly unpredictable and likely depending on the degree of surface contamination of the substrate. A parallel systematic resonant Raman study is performed ranging from one to five layers clearly exhibiting systematic layer dependent spectral features in the one-five layers range. For the first time a layer estimation number based on a quantitative analysis of resonant Raman and PL spectra is proposed.

Cellulose derivatives have many potential applications in the field of biomaterials and composites, in addition to several ways of modification leading to them. Silanization in aqueous media is one of the most promising routes to create multipurpose and organic–inorganic hybrid materials. Silanization has been widely used for cellulosic and nano-structured celluloses, but was a problem so far if to be applied to the common cellulose derivative “dialdehyde cellulose” (DAC), i.e., highly periodate-oxidized celluloses. In this work, a straightforward silanization protocol for dialdehyde cellulose is proposed, which can be readily modified with (3-aminopropyl)triethoxysilane. After thermal treatment and freeze-drying, the resulting product showed condensation and cross-linking, which was studied with infrared spectroscopy and ¹³C and ²⁹Si solid-state nuclear magnetic resonance (NMR) spectroscopy. The cross-linking involves both links of the hydroxyl group of the oxidized cellulose with the silanol groups (Si-O-C) and imine-type bonds between the amino group and keto functions of the DAC (-HC=N-). The modification was achieved in aqueous medium under mild reaction conditions. Different treatments cause different levels of hydrolysis of the organosilane compound, which resulted in diverse condensed silica networks in the modified dialdehyde cellulose structure.

Oxidation of cellulose with periodate under aqueous conditions yields dialdehyde cellulose, a promising functional cellulose derivative. The main obstacles for this oxidation have been its slow kinetics and the dilute reaction conditions, requiring considerable amounts of water and energy. In this study, these drawbacks are overcome by conducting the oxidation at high cellulosic pulp consistency with a cellulose/water weight ratio of 1:4. The oxidizer, cellulose, and water are efficiently mixed in a ball mill. Oxidation occurs mostly in the subsequent step, during the resting time (no further milling/mixing is required). The reaction and resource efficiency of the process are optimized by experimental design and a maximum aldehyde content of 8 mmol g⁻¹ is obtained with a periodate/cellulose molar ratio of 1.25, a milling time of 2 min, and a resting time of 8 h. The developed method allows fine tuning of the oxidation level and is a key step towards the sustainable periodate oxidation of cellulose also on larger scale.

The traditional binder used in mineral wool is phenolic resin that makes mineral wool insulations reliable and efficient. The toxicity and health hazards of phenol and formaldehyde are becoming more and more pressing, and the industrial production needs to focus on safer precursors. Several formulations of bio-based binders for mineral wool have been developed, meeting the challenge of performing equally well as conventional binders. Technical lignins, due to their intrinsic structure and their abundance, are good candidates for future industrial adhesives. Carbohydrates are other class of biomaterials widely used in both research and patent formulations toward mineral wool binders. Proteins and cardanol are still largely unknown precursors, although they have hidden potentials for reliable binder systems. Even if conventional binders are not replaced completely with bio-based alternatives today, a partial use is already a step forward in the right direction – toward future biorefinery-based industries and knowledge-based bioeconomies in general.

Localized strained silicon was observed with a suitable resolution in a real semiconductor device by tip-enhanced Raman spectroscopy (TERS). The device was made via a standard industrial process and its silicon trench isolation structures were used for the silicon strain analysis obtaining results according to finite element method-based simulation data. We have achieved a reliable and repeatable enhancement factor obtaining a trace of strained silicon along the structure with suitable nanometer spatial resolution compatible with IC industry requirements. We demonstrate that the complexity to analyze a real 3D structure, directly from the production lines and not ad hoc realized, entails the challenges to individuate the optimal tip shape, tip contact angle, tip composition, tip positioning system, laser power, and wavelength to achieve an appropriate plasmon resonance inducing a relevant signal to noise ratio. This work gives the base to address the development in TERS optimization for real industrial applications.