Cervical cancer remains a significant global health burden, highlighting the need for more effective tools for early detection and tissue characterization. In this study, we propose a multimodal strategy that combines Raman spectroscopy, Atomic Force Microscopy (AFM), and Scanning Electron Microscopy (SEM) to investigate the molecular and morphological features of cervical squamous cell carcinoma (SCC). Raman spectroscopy was used to analyze biochemical signatures across different tissue regions tumor, necrotic, stromal, and glandular within the 813-1668 cm-1 range, identifying distinct molecular profiles between malignant and healthy areas. Specific vibrational peaks associated with DNA, proteins, and lipids were examined to track molecular changes related to tumor progression. AFM enabled nanoscale mapping of surface morphology, revealing structural irregularities associated with malignancy, while SEM provided detailed imaging of cellular and extracellular architecture, enhancing the visualization of cancer-induced morphological alterations. Although Raman spectroscopy has been studied for decades in cancer research, it has not yet replaced Pap smears and biopsies in clinical practice due to challenges in standardization, reproducibility, and clinical validation. This pilot study aims to serve as a stepping stone toward that goal, providing proof-of-concept data that may support the gradual translation of Raman spectroscopy into clinically relevant diagnostic workflows and underscores the potential of the technique, supported by complementary high-resolution imaging techniques, in the characterization of cervical cancer tissues. The integration of Raman, AFM, and SEM was used here as a pilot approach on paraffin-embedded samples, with AFM and SEM providing supportive morphological information while the long-term aim is to transfer Raman spectroscopy to fresh, untreated tissues, where its non-destructive and label-free nature could enable minimally invasive diagnostic applications.

Biofouling arises from non-specific adsorption of several components present in complex biofluids, such as full blood, on the surface of electrochemical biosensors, with a resulting loss of functionality. Most biomarkers of clinical relevance are present in biological fluids at extremely low concentrations, making antibiofouling strategies necessary in electrochemical biosensing. Here, we demonstrate the effect of a highly porous gold (h-PG) film electrodeposited on a gold screen-printed electrode (AuSPE) using a self-templated method via hydrogen bubbling as an antibiofouling strategy in electrochemical biosensor development following exposure of the electrode to bovine serum albumin (BSA) at two different concentrations (2 and 32 mg/mL). The h-PG film has a high electrochemically active surface area, 88 times higher than the AuSPE electrode, with a pore size ranging from 2 to 50 μm. A rapid decrease in the Faradaic current was observed with the unmodified AuSPE, attesting to the strong biofouling effect of BSA at both concentrations tested. Notably, the h-PG-modified electrode showed an initial peak current decline, more evident at a higher BSA concentration, followed by rapid electrode regeneration when the electrode was left idle in the biofouling solution. Similar results were obtained for unmodified and modified electrodes in real serum and plasma samples. The regeneration process, explained in terms of balance between h-PG pore size and protein size, the nanoscale architecture of the h-PG electrodes, and repulsive electrostatic forces, indicates the huge potential of the h-PG film for use in biomedical electrochemical sensing.

Abstract Understanding and decoupling the effects of strain and doping in graphene remains a central challenge in Raman spectroscopy, as far-field measurements inherently average local variations. In this work, we combine conventional Raman spectroscopy, tip-enhanced Raman spectroscopy (TERS), G–2D bands correlation analysis, and principal component analysis (PCA) to investigate graphene grown on copper (Cu) and transferred onto silicon (Si) substrates, with the aim of probing substrate-dependent spectral variability across different length scales. Far-field Raman measurements show distinct but relatively compact spectral distributions for graphene on Cu and Si, with trends that can be qualitatively associated with mixed strain- and dopinglike contributions. These measurements primarily reflect a spatially averaged response, which masks local variations. In contrast, TERS reveals a significantly broader and spatially heterogeneous spectral behavior, particularly for graphene on Cu, whereas graphene on Si exhibits a more compact distribution. These differences indicate that substrate-dependent interactions and transfer processes influence not only the average spectral response but also its local variability. Correlation analysis based on G–2D trends provides a qualitative framework to identify dominant spectral tendencies, while PCA enables a data-driven description of spectral variability without relying on peak fitting. PCA distinguishes the main substrate-dependent contribution from additional sources of variability and, through spatial mapping of principal components, reveals that these variations are spatially structured at the nanoscale in TERS measurements, whereas Raman maps remain comparatively smooth. Overall, the combined approach demonstrates that TERS does not simply enhance the Raman signal locally but provides access to the distribution of local spectral variations that are averaged out in far-field measurements. This methodology offers a robust framework for the nanoscale investigation of graphene and can be extended to other two-dimensional materials, where local heterogeneity plays a key role in determining macroscopic properties.

Despite the recognized therapeutic potential of Rosmarinic Acid (RA), its clinical use remains limited due to poor water solubility, chemical instability, and rapid mucociliary clearance following intranasal administration. To address these limitations, two different nanocarriers: Solid Lipid Nanoparticles (SLNs) and oil-in-water nanoemulsions (O/W NEs) were designed, prepared and characterized, to improve the intranasal delivery and therapeutic efficacy of RA in allergic rhinitis. These nanosystems were optimized to encapsulate RA, enhancing its solubility and enabling controlled release. To prolong residence time at the nasal mucosa, chitosan was introduced in RA-based NEs as mucoadhesive polymer. A comprehensive physicochemical characterization was carried out, including evaluation of size, zeta potential, membrane fluidity, and structural organization. Stability was assessed under storage and physiologically conditions. In particular, Atomic Force Microscopy (AFM) and Small-Angle X-ray Scattering (SAXS) analyses were conducted to gain deeper insights into the formulations surface morphology and internal nanostructure. Obtained results confirmed the ability of both systems to protect RA from degradation and promote sustained release. Mucoadhesion studies demonstrated the interaction of the chitosan-coated NEs with mucin, increasing retention on the nasal mucosa. Among the two formulations, SLN-RA was selected for nasal spray development and extensively characterized, including resistance to nebulization, droplet size distribution, and microbiological and pharmacological studies, to evaluate its suitability for intranasal administration. The results confirmed that the SLN-based nasal spray maintained favorable physicochemical and mucoadhesive properties, ensuring efficient delivery to the upper respiratory tract. Biological assays revealed that encapsulated RA retained its antioxidant and anti-inflammatory properties, reducing the expression of inflammatory markers such as High Mobility Group Box 1 (HMGB1). Altogether, these findings suggest that SLNs represent the best and promising carrier for the non-invasive delivery of RA in the nasal cavity. Their integration into nasal spray formulations could offer an effective therapeutic strategy for allergic rhinitis and other inflammatory conditions of the upper respiratory tract.

During the Roman period, amphorae were essential for storing and transporting goods, especially food. This study examines a fragment of a Roman amphora with a red titulus pictus, discovered at the Poggio Moscini archaeological site (Bolsena, Italy) and dated between 150 and 100 BC. A comprehensive archaeometric study has been conducted using the non-disruptive techniques of X-ray microscopy (XRM), X-ray powder diffraction (XRPD), energy-dispersive X-ray fluorescence (ED-XRF) spectroscopy, fiber optics reflectance spectroscopy (FORS) and micro-Raman spectroscopy. XRM revealed a preferential pore orientation consistent with wheel-throwing manufacture. XRPD identified quartz, diopside, gehlenite, anorthite and sanidine, indicating the use of Ca-rich clays and firing temperatures between similar to 900 and 1000 degrees C. ED-XRF demonstrated a similar composition between the ceramic body and the pigment, confirming Fe-rich clay and Fe-oxide-based pigmentation. FORS shows absorption features typical of hematite, and micro-Raman spectroscopy identifies hematite as the red pigment and rules out gypsum in the ceramic body.

The rational design of selective Cu-based electrocatalysts for CO2 electroreduction requires an understanding of how dopants modify catalytic pathways under realistic conditions. However, the active surface often evolves dynamically during electrolysis, hindering direct comparison between theoretical predictions and experimental selectivity. Herein, we investigate how dopant redox stability influences reaction pathways on Cu by combining controlled sputter-based synthesis of Ti- and Sn-modified Cu thin films with electrochemical measurements and dispersion-corrected density functional theory (DFT-D) within the computational hydrogen electrode framework. Composition-spread electrodes enable systematic comparison of dopant effects, while DFT-D quantifies how Ti and Sn modify the thermodynamics of key intermediates (H*, COOH*, CO*, and OCHO*). Experiments reveal that Ti-modified Cu favors hydrogen evolution, whereas Sn-modified Cu produces CO with unaccounted charge consistent with liquid products. Post-electrolysis XRD shows TiO2 formation on Cu@Ti and Cu3Sn intermetallic phases on Cu@Sn, indicating distinct phase evolution during reaction. Combined experimental-theoretical analysis reveals a stability-selectivity relationship in doped Cu catalysts: oxophilic Ti oxidizes into HER-active oxide motifs, whereas redox-stable Sn forms metallic or intermetallic environments that stabilize O-bound intermediates and promote CO/formate pathways. This experimentally validated framework provides a transferable guideline for designing Cu-based CO2 reduction catalysts and may enable future high-throughput screening of dopant chemistries.

This study focuses on chemical and microstructural results on four bronze artifacts, dating back to the 3rd-4th centuries AD. These artifacts were unearthed in the archaeological site of the Roman Cistern at Spoletino (Civitella D'Agliano, VT, Central Italy). They were studied using a Reflected Light Microscope, micro-Raman spectroscopy, SEM-EDS analysis, and cluster analysis, providing reliable and complementary data on the samples. SEM-EDS results indicated the use of different Cu alloys at the Roman site. Lead was added to improve the fluidity of the molten bronze in the locked item, while scrap metal containing Zn and leaded bronze were mixed to produce gunmetal and furniture accessories. A binary Cu-Sn alloy was employed for decorative and cosmetic objects. The corrosion products, identified by micro-Raman spectroscopy, are cuprite (Cu2O), malachite (Cu2(OH)2CO3), hydrocerussite (Pb3(CO3)2(OH)2), and libethenite (Cu2(OH)PO4), reflecting interactions with burial environments. Cluster analysis simplified the interpretation of complex Raman maps, especially in samples with multifaceted corrosion processes that involved overlapping phases. The data confirmed the absence of chloride ions on the patinas and extensive decuprification processes on the external surface, with the diffusion of environmental elements, such as phosphates, towards the bulk metal. A strong correlation was observed between fractured paths and corrosion patterns along artifact edges.

In this study, we combined experimental Piezoresponse Force Microscopy (PFM) analysis with an empirically corrected Furukawa model to predict the piezoelectric behavior of Poly(Vinylidene Fluoride-co-Trifluoroethylene) (PVDF-TrFE) films functionalized with CoFe2O4 (CFO) Magnetic Nanoparticles (MNPs). According to our empirical model, the piezoelectric response observed from PFM analysis on the PVDF-TrFE/CFO films was mainly influenced by the interaction between the CFO MNPs and the polymer active β phase of the polymer, providing a high piezoelectric coefficient d33 ( 6.5 pm/V) at a low CFO concentration of 5 wt

Toxic substances are often employed in conventional stone preservation techniques, whereas biorestoration offers material compatibility along with significant benefits for cultural heritage preservation, environmental safety, and sustainability. However, the application of this innovative technique to natural rocks is not fully understood. In this study, we evaluated the efficiency of a carbonatogenic bacterial strain (Lysinbacillus fusiformis 3.20) on three natural carbonate rocks: Calcarenite (CA), Travertine (TR) and Marble (MA), having different porosities. We integrated surface analyses (Field Emission Scanning Electron Microscopy, Atomic Force Microscopy, and X-Ray Diffraction) with bulk analyses (Porosity, Ultrasonic Wave Velocity, and Dynamic Elastic Moduli) to investigate the bioconsolidation processes. The results indicated that the biomineralization treatment had no effect on MA samples, while it improved the physical and mechanical properties of both CA and TR, evidenced by the formation of new bioprecipitates. Total and effective porosity decreased, particularly in CA, while ultrasonic wave velocities (Vp and Vs) and Young's modulus increased, with Poisson's ratio remaining unchanged. Comparative observations suggest that connected, randomly distributed, and low aspect ratio pores facilitate microbial activity by enabling deeper bacterial penetration into the stone, supporting nutrient distribution and the formation of calcium carbonate precipitates. When the treatment is effective, stiffness and strength are expected to increase due to reduced effective porosity, while resistance to shear deformation remains nearly constant, as does the relationship between porosity and wave velocities.

A novel ecofriendly electrochemical sensor for in-situ detection of testosterone based on gold nanoparticles (AuNPs) and a semi-amorphous metal organic framework (MOF) has been developed for clinical diagnosis and doping control. For this purpose, MIL-100(Fe) has been synthetized according to a green path with crystallization times tuned in the range 2–24 h. The sensor platform was constructed via drop-casting MOF and AuNPs onto a graphene (GPH) screen-printed electrode (SPE) surface. The surface structure and morphology and the electrochemical properties of unmodified and modified electrodes were investigated by (SEM), energy-dispersive X-ray spectroscopy analysis (EDX), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), demonstrating the enhanced electrochemical response of the platform modified with MOF obtained with the shorter crystallization time of 2 h (MOF2h) and AuNPs, compared to unmodified electrode. The AuNPs/MOF2h/GPH/SPE based sensor was responsive to nanomolar concentrations of testosterone, showing a wide linear range from 1 to 50 nM and a detection limit (LOD) of 0.5 nM, which correlates to the serum concentration values of healthy males. The combination of these results with the excellent performance maintained by the proposed sensor when interfaced with a miniaturized potentiostat (Sensit-Smart) directly connected to a smartphone, highlights the potential of this device towards in-situ electrochemical testosterone sensing, in particular for medical diagnosis and for doping control.

Reliable characterization techniques that guarantee real-time quality control with a non-destructive and multiscale approach are currently an essential necessity for electronic industries. Tip-Enhanced Raman Spectroscopy (TERS) offers an excellent solution to this demand. In addition to providing chemical composition through the Raman spectrometer, TERS leverages the high lateral resolution of the coupled Atomic Force Microscope, enabling chemical and morphological characterization of samples down to the nanometer scale. This study advances the application of TERS by employing ad-hoc prepared TiN-coated probes, engineered to operate in cleanrooms while guaranteeing remarkable performances in terms of electromagnetic field enhancement. The subject of this analysis is a strained-silicon-based device, a technology meant to enhance the carrier's mobility in Complementary Metal-Oxide-Semiconductor (CMOS) architectures. The goal of the characterization is to detect the strain induced by a thin Si1-xGex alloy grown on a Si(100) substrate in the silicon lattice. TERS enables not only the detection of strain in the crystal structure but also its magnitude at different levels of depth, despite the penetration depth of the laser employed. This study is a result of the activities carried out in the framework of the European Union founded project CHALLENGES included in the Horizon2020 program.

Heterojunction (HJT) photovoltaic cells represent a significant advancement in solar technology due to their ability to combine high efficiency with durability. However, the integration of shingling technology, a process which employs precise laser cutting to maximize panel performance, introduces substantial challenges. The utilization of nanosecond infrared (ns-IR) lasers for segmentation often results in structural and morphological damage, particularly along the cut edges, thereby impacting the optical, mechanical, and electrical properties of the cells. This study employs advanced multi-scale characterisation techniques, including scanning electron microscopy (SEM), Raman spectroscopy, photoluminescence (PL) analysis, and atomic force microscopy (AFM), to investigate these laser-induced defects. The results reveal extensive disruptions to the surface morphology, including the formation of silicon oxide residues and deformation of pyramidal structures essential for light trapping. Raman and PL analyses highlight strain and disorder within the silicon lattice, particularly near the cut edges, where defects reduce crystalline quality and increase recombination losses. Additionally, Kelvin Probe Force Microscopy (KPFM) measurements indicate a significant decline in surface potential and work function, extending up to millimeters from the cut region, further compromising cell efficiency. These findings emphasize the critical need to optimize laser cutting processes for HJT cells, particularly in shingling applications. Achieving this objective necessitates minimizing defects and preserving the integrity of silicon and indium tin oxide layers, thereby facilitating the fabrication of high-performing solar cells that can be scaled up for application in more efficient and reliable photovoltaic solutions.

The use of engineered nanomaterials is widely distributed throughout the whole food chain to improve yield, durability, taste, and appearance of commercialized food. Moreover, nanotechnology stepped into the world of food packaging, granting better conservation of foods, avoiding bacterial contaminations, or reducing the spoiling of nutritive substances. All these improvements, however, need to be achieved in a ‘safe’ way, thus there is a wide and constantly updated legislation that deals with the possible toxicity of these additions by posing some limitation to the percentage of nanosized elements added and to their composition. Thus, the characterization of the nanomaterials ‘in situ’, e.g., directly inside the biological matrix, is of paramount importance, to measure the real concentration of the nanomaterials as well as their distribution and unwanted local modification of the biological matrix. Here we review the main high-resolution techniques that are currently used for these characterizations in combination with the most up-to-date analytical methods, i.e., X-ray (X-ray microscopy and X-ray diffraction), scanning microscopies (electron microscopy and atomic force microscopy), optical spectroscopies (infrared spectroscopy and Raman spectroscopy), and mass spectrometry, discussing their benefits and drawbacks. Some important results are reported and their applications are discussed not only in the characterization of nanosized objects deliberately added to the food and food packaging to improve their properties, but also in the characterization of unwanted nano-sized and micro-sized objects that originate from possible environmental contamination that can happen at every step of the food chain starting from water. Among them, the characterization of micro- and nano-plastics and some nanosized metallic pollutants using these analytical techniques is discussed.

The characterization of nanoparticles (NPs) has become increasingly important due to their wide-ranging applications in fields such as biomedicine and drug delivery. NPs have emerged as promising candidates for drug delivery systems due to their unique physicochemical properties, which enable them to interact with biological systems at the molecular level. Among these, soft nanocarriers, such as niosomes, and hard nanocarriers, such as Iron Oxide Nanoparticles (IONPs), offer distinct advantages for targeted therapy and diagnostics. This study provides a comprehensive, multi-disciplinary evaluation of two distinct types of nanoparticles: soft nanocarriers (niosomes, NVs) and hard nanocarriers (IONPs), by examining their physicochemical properties, cellular uptake, and cytotoxicity profiles. This comparative analysis seeks to highlight the different behaviour of soft and hard nanoparticles in drug delivery applications, with a particular focus on the impact of surface modifications. The addition of chitosan to sample NVsB not only resulted in an increase in particle dimensions but also shifted the ζ-potential to positive values which could enhance the interactions with cell membranes, improving cellular uptake. As desired, the obtained ζ-potential value of NVsB-Chit was comparable to that of the commercial coated ferrofluid. In addition to the traditional characterization techniques, this study integrates advanced analytical methods, such as Atomic Force Microscopy (AFM), complementing traditional techniques such as Dynamic Light Scattering (DLS), to assess the nanoscale topography of both types of nanoparticles. Cytotoxicity studies on Calu-3 lung adenocarcinoma cells were conducted to evaluate the biocompatibility of the nanoparticles, demonstrating that NVs and FluidMAG exhibited minimal cytotoxic effects, particularly at lower concentrations. Cell internalization was confirmed for IONPs by magnetic cell separation whereas confocal microscopy analysis has been conducted for calcein-loaded NVs intracellular visualization. By integrating structural, chemical, and biological evaluations, we take an interdisciplinary approach which could also enable us to explore how variations in nanoparticle design (such as surface charge, size and coating) affect their performance in drug delivery and diagnostics. Moreover, combining physicochemical characterizations (e.g., hydrodynamic diameter, zeta potential and nanoparticles morphology) with biological evaluations (e.g., cellular uptake and safety profiles) allows for a holistic assessment of these nanocarriers to gain a comprehensive understanding of their behaviour and performance. This aspect is crucial for designing more efficient, safer, and targeted nanomedicines.

The identification of blue pigments in Roman wall paintings provides crucial insights into the materials, artistic techniques, and trade routes in the antiquity. The present study focuses on the analysis of a blue pigment lump discovered at Ponticello (Bolsena, Italy) initially thought to be Egyptian blue. The lump pigment is compared with two synthetic ultramarine pigments (Poggi and Divolo), "Herculaneum blue," Egyptian blue, and natural lapis lazuli from Monte Somma, Italy. Through a multi-analytical approach that comprehends energy-dispersive X-ray fluorescence (ED-XRF) spectroscopy, micro-Raman spectroscopy, and X-ray powder diffraction (XRPD), the pigment was univocally identified as natural lazurite, the primary component of lapis lazuli. Chemometrics, including principal component analysis (PCA), was applied to the ED-XRF data to reveal patterns in the elemental composition of the samples. This finding is significant as ultramarine blue was a rare and expensive material in Roman times, which was traditionally sourced from distant regions like Afghanistan. While this study does not aim to determine the geographical provenance of the pigment, it offers important insights into Roman artistic practices, economic resources, and trade networks. Future research will explore the chemical composition of the pigments present in the frescoes from the archaeological area of Volsinii to provide important further insights into ancient material exchanges.

Tip enhanced Raman spectroscopy (TERS) increases the spatial resolution of Raman spectroscopy to the nanoscale. The potentiality of TERS is demonstrated on single milk derived extracellular vesicles, allowing the nanoscale chemical investigation of their lipid membrane.

The semiconductor industry is undergoing a transformative phase, marked by the relentless drive for miniaturization and a constant demand for higher performance and energy efficiency. However, the reduction of metal–oxide–semiconductor field-effect transistor sizes for advanced technology nodes below 10 nm presents several challenges. In response, strained silicon technology has emerged as a key player, exploiting strain induction in the silicon crystal lattice to improve device performance. At the same time, there has been a growing need for characterization techniques that allow in-line monitoring of sample conditions during semiconductor manufacturing, as an alternative to traditional methods such as transmission electron microscopy or high-resolution X-ray diffraction, which have several limitations in terms of measurement time and sample destructiveness. This paper explores the application of advanced spectroscopic characterization techniques, in particular µ-Raman spectroscopy and tip-enhanced Raman spectroscopy (TERS), to meet the evolving needs of the semiconductor industry for quality control and failure analysis, increasingly requiring faster and non-destructive characterization techniques. µ-Raman provides insight into strain values and distributions of strained layers with different thicknesses and germanium concentrations, but its lateral resolution is constrained by the Abbe diffraction limit. TERS, on the other hand, emerges as a powerful non-destructive technique capable of overcoming diffraction limits by exploiting the combination of an atomic force microscope with a Raman spectrometer. This breakthrough makes it possible to estimate the chemical composition and induced strain in the lattice by evaluating the Raman peak position shifts in strained and unstrained silicon layers, providing crucial insights for nanoscale strain control. In particular, this paper focuses on the TERS characterization of Si 0.7 Ge 0.3 epitaxial layers grown on a silicon-on-insulator device, demonstrating the effectiveness of this technique and the high lateral resolution that can be achieved.

Carbon nanostructures are highly promising materials for applications in a variety of different fields. Besides their interesting performances, the possibility to synthesize them from biowaste makes them an eco-friendly resource widely exploitable within a circular economy context. The present work deals with the green, one-pot synthesis of graphene quantum dots (GQDs) from carbon aerogels (CAs) derived from rice husk (RH). After having obtained CAs upon purification of RH, followed by gelification and carbonization of the resulting cellulose, the one-pot solventless production of GQDs was obtained by ball milling. This method determined the formation of crystalline nanostructures with a diameter of around 20 nm, which were analyzed via scanning electron microscopy, transmission electron microscopy, atomic force microscopy, X-ray diffraction, and Raman spectroscopy to obtain a full morphological and structural characterization. GQDs were used as electrode materials for supercapacitors and Li-ion batteries, showing the ability to both accumulate charges over the surface and intercalate lithium-ions. The reported results are a proof of principle of the possibility of exploiting GQDs as support material for the development of advanced systems for energy storage.