Streptomyces coelicolor Vesicles: Many Molecules To Be Delivered.

Streptomyces coelicolor is a model organism for the study of Streptomyces, a genus of Gram-positive bacteria that undergoes a complex life cycle and produces a broad repertoire of bioactive metabolites and extracellular enzymes. This study investigated the production and characterization of membrane vesicles (MVs) in liquid cultures of S. coelicolor M145 from a structural and biochemical point of view; this was achieved by combining microscopic, physical and -omics analyses. Two main populations of MVs, with different sizes and cargos, were isolated and purified. S. coelicolor MV cargo was determined to be complex, containing different kinds of proteins and metabolites. In particular, a total of 166 proteins involved in cell metabolism/differentiation, molecular processing/transport, and stress response were identified in MVs, the latter functional class also being important for bacterial morpho-physiological differentiation. A subset of these proteins was protected from degradation following treatment of MVs with proteinase K, indicating their localization inside the vesicles. Moreover, S. coelicolor MVs contained an array of metabolites, such as antibiotics, vitamins, amino acids, and components of carbon metabolism. In conclusion, this analysis provides detailed information on S. coelicolor MVs under basal conditions and on their corresponding content, which may be useful in the near future to elucidate vesicle biogenesis and functions. IMPORTANCE Streptomycetes are widely distributed in nature and characterized by a complex life cycle that involves morphological differentiation. They are very relevant in industry because they produce about half of all clinically used antibiotics, as well as other important pharmaceutical products of natural origin. Streptomyces coelicolor is a model organism for the study of bacterial differentiation and bioactive molecule production. S. coelicolor produces extracellular vesicles that carry many molecules, such as proteins and metabolites, including antibiotics. The elucidation of S. coelicolor extracellular vesicle cargo will help us to understand different aspects of streptomycete physiology, such as cell communication during differentiation and response to environmental stimuli. Moreover, the capability of these vesicles for carrying different kinds of biomolecules opens up new biotechnological possibilities related to drug delivery. Indeed, decoding the molecular mechanisms involved in cargo selection may lead to the customization of extracellular vesicle content.

Luminescence mechanisms of defective ZnO nanoparticles.

ZnO nanoparticles (NPs) synthesized by pulsed laser ablation (PLAL) of a zinc plate in deionized water were investigated by time-resolved photoluminescence (PL) and complementary techniques (TEM, AFM, µRaman). HRTEM images show that PLAL produces crystalline ZnO NPs in wurtzite structure with a slightly distorted lattice parameter a. Consistently, optical spectra show the typical absorption edge of wurtzite ZnO (Eg = 3.38 eV) and the related excitonic PL peaked at 3.32 eV with a subnanosecond lifetime. ZnO NPs display a further PL peaking at 2.2 eV related to defects, which shows a power law decay kinetics. Thermal annealing in O2 and in a He atmosphere produces a reduction of the A1(LO) Raman mode at 565 cm(-1) associated with oxygen vacancies, accompanied by a decrease of defect-related emission at 2.2 eV. Based on our experimental results the emission at 2.2 eV is proposed to originate from a photo-generated hole in the valence band recombining with an electron deeply trapped in a singly ionized oxygen vacancy. This investigation clarifies important aspects of the photophysics of ZnO NPs and indicates that ZnO emission can be controlled by thermal annealing, which is important in view of optoelectronic applications.

Visible-ultraviolet vibronic emission of silica nanoparticles.

We report the study of the visible-ultraviolet emission properties and the structural features of silica nanoparticles prepared through a laboratory sol-gel technique. Atomic force microscopy, Raman and Infrared investigations highlighted the 10 nm size, purity and porosity of the obtained nanoparticles. By using time resolved photoluminescence techniques in air and in a vacuum we were able to single out two contributions in the visible emission: the first, stable in both atmospheres, is a typical fast blue band centered around 2.8 eV; the second, only observed in a vacuum around the 3.0-3.5 eV range, is a vibrational progression with two phonon modes at 1370 cm(-1) and 360 cm(-1). By fully characterizing the spectroscopic features of this structured emission, we determine its vibronic properties and clarify the different origins with respect to the blue luminescent defect.

Defects in epitaxial 4H-SiC revealed by exciton recombination.

In this work, we conducted an analysis of 4H-SiC epitaxial layer grown on two distinct 4H-SiC substrates (both 6 inches in diameter) using non-invasive techniques such as micro-Raman spectroscopy, steady-state absorption spectroscopy and time-resolved photoluminescence spectroscopy. We have shown that despite the doping homogeneity, confirmed by micro-Raman and steady-state absorption spectroscopy, the carrier lifetime, assessed by monitoring the excitonic band at 3.2 eV by time-resolved photoluminescence spectroscopy, depends on the position on the wafer. This variability is attributed to the presence of defects, such as impurities or point defects, which are not uniformly distributed on the epitaxial layer and that, in addition to extended defects, affect the charge carrier recombination. Additionally, it is found that interactions with the underlying substrate could contribute to these effects as evidenced in regions of the substrate characterized by differences of doping.

Unveiling the MIL-53(Al) MOF: Tuning Photoluminescence and Structural Properties via Volatile Organic Compounds Interactions.

MIL-53(Al) is a metal-organic framework (MOF) with unique properties, including structural flexibility, thermal stability, and luminescence. Its ability to adsorb volatile organic compounds (VOCs) and water vapor makes it a promising platform for sensing applications. This study investigated the adsorption mechanism of MIL-53(Al) with different VOCs, including ketones, alcohols, aromatics, and water molecules, focusing on structural transformations due to pore size variation and photoluminescence properties. The reported results assess MIL-53(Al) selectivity towards different VOCs and provide insights into their fundamental properties and potential applications in sensing.

Interface Properties of MoS2 van der Waals Heterojunctions with GaN.

The combination of the unique physical properties of molybdenum disulfide (MoS2) with those of gallium nitride (GaN) and related group-III nitride semiconductors have recently attracted increasing scientific interest for the realization of innovative electronic and optoelectronic devices. A deep understanding of MoS2/GaN interface properties represents the key to properly tailor the electronic and optical behavior of devices based on this heterostructure. In this study, monolayer (1L) MoS2 was grown on GaN-on-sapphire substrates by chemical vapor deposition (CVD) at 700 °C. The structural, chemical, vibrational, and light emission properties of the MoS2/GaN heterostructure were investigated in detail by the combination of microscopic/spectroscopic techniques and ab initio calculations. XPS analyses on as-grown samples showed the formation of stoichiometric MoS2. According to micro-Raman spectroscopy, monolayer MoS2 domains on GaN exhibit an average n-type doping of (0.11 ± 0.12) × 1013 cm-2 and a small tensile strain (ε ≈ 0.25%), whereas an intense light emission at 1.87 eV was revealed by PL analyses. Furthermore, a gap at the interface was shown by cross-sectional TEM analysis, confirming the van der Waals (vdW) bond between MoS2 and GaN. Finally, density functional theory (DFT) calculations of the heterostructure were carried out, considering three different configurations of the interface, i.e., (i) an ideal Ga-terminated GaN surface, (ii) the passivation of Ga surface by a monolayer of oxygen (O), and (iii) the presence of an ultrathin Ga2O3 layer. This latter model predicts the formation of a vdW interface and a strong n-type doping of MoS2, in closer agreement with the experimental observations.

Multiscale Investigation of the Structural, Electrical and Photoluminescence Properties of MoS2 Obtained by MoO3 Sulfurization.

In this paper, we report a multiscale investigation of the compositional, morphological, structural, electrical, and optical emission properties of 2H-MoS2 obtained by sulfurization at 800 °C of very thin MoO3 films (with thickness ranging from ~2.8 nm to ~4.2 nm) on a SiO2/Si substrate. XPS analyses confirmed that the sulfurization was very effective in the reduction of the oxide to MoS2, with only a small percentage of residual MoO3 present in the final film. High-resolution TEM/STEM analyses revealed the formation of few (i.e., 2-3 layers) of MoS2 nearly aligned with the SiO2 surface in the case of the thinnest (~2.8 nm) MoO3 film, whereas multilayers of MoS2 partially standing up with respect to the substrate were observed for the ~4.2 nm one. Such different configurations indicate the prevalence of different mechanisms (i.e., vapour-solid surface reaction or S diffusion within the film) as a function of the thickness. The uniform thickness distribution of the few-layer and multilayer MoS2 was confirmed by Raman mapping. Furthermore, the correlative plot of the characteristic A1g-E2g Raman modes revealed a compressive strain (ε ≈ -0.78 ± 0.18%) and the coexistence of n- and p-type doped areas in the few-layer MoS2 on SiO2, where the p-type doping is probably due to the presence of residual MoO3. Nanoscale resolution current mapping by C-AFM showed local inhomogeneities in the conductivity of the few-layer MoS2, which are well correlated to the lateral changes in the strain detected by Raman. Finally, characteristic spectroscopic signatures of the defects/disorder in MoS2 films produced by sulfurization were identified by a comparative analysis of Raman and photoluminescence (PL) spectra with CVD grown MoS2 flakes.

Intrinsic Point Defects in Silica for Fiber Optics Applications.

Due to its unique properties, amorphous silicon dioxide (a-SiO2) or silica is a key material in many technological fields, such as high-power laser systems, telecommunications, and fiber optics. In recent years, major efforts have been made in the development of highly transparent glasses, able to resist ionizing and non-ionizing radiation. However the widespread application of many silica-based technologies, particularly silica optical fibers, is still limited by the radiation-induced formation of point defects, which decrease their durability and transmission efficiency. Although this aspect has been widely investigated, the optical properties of certain defects and the correlation between their formation dynamics and the structure of the pristine glass remains an open issue. For this reason, it is of paramount importance to gain a deeper understanding of the structure-reactivity relationship in a-SiO2 for the prediction of the optical properties of a glass based on its manufacturing parameters, and the realization of more efficient devices. To this end, we here report on the state of the most important intrinsic point defects in pure silica, with a particular emphasis on their main spectroscopic features, their atomic structure, and the effects of their presence on the transmission properties of optical fibers.

Micro-photoluminescence of Carbon Dots Deposited on Twisted Double-Layer Graphene Grown by Chemical Vapor Deposition.

Carbon-based nanomaterials, such as carbon dots (CDs) and graphene (Gr), feature outstanding optical and electronic properties. Hence, their integration in optoelectronic and photonic devices is easier thanks to their low dimensionality and offers the possibility to reach high-quality performances. In this context, the combination of CDs and Gr into new nanocomposite materials CDs/Gr can further improve their optoelectronic properties and eventually create new ones, paving the way for the development of advanced carbon nanotechnology. In this work, we have thoroughly investigated the structural and emission properties of CDs deposited on single-layer and bilayer graphene lying on a SiO2/Si substrate. A systematic Raman analysis points out that bilayer (BL) graphene grown by chemical vapor deposition does not always respect the Bernal (AB) stacking, but it is rather a mixture of twisted bilayer (t-BL) featuring domains with different twist angles. Moreover, in-depth micro-photoluminescence measurements, combined with atomic force microscopy (AFM) morphological analysis, show that CD emission efficiency is strongly depleted by the presence of graphene and in particular is dependent on the number of layers as well as on the twist angle of BL graphene. Finally, we propose a model which explains these results on the basis of photoinduced charge-transfer processes, taking into account the energy levels of the hybrid nanosystem formed by coupling CDs with t-BL/SiO2.

Strain, Doping, and Electronic Transport of Large Area Monolayer MoS2 Exfoliated on Gold and Transferred to an Insulating Substrate.

Gold-assisted mechanical exfoliation currently represents a promising method to separate ultralarge (centimeter scale) transition metal dichalcogenide (TMD) monolayers (1L) with excellent electronic and optical properties from the parent van der Waals (vdW) crystals. The strong interaction between Au and chalcogen atoms is key to achieving this nearly perfect 1L exfoliation yield. On the other hand, it may significantly affect the doping and strain of 1L TMDs in contact with Au. In this paper, we systematically investigated the morphology, strain, doping, and electrical properties of large area 1L MoS2 exfoliated on ultraflat Au films (0.16-0.21 nm roughness) and finally transferred to an insulating Al2O3 substrate. Raman mapping and correlative analysis of the E' and A1' peak positions revealed a moderate tensile strain (ε ≈ 0.2%) and p-type doping (n ≈ -0.25 × 1013 cm-2) of 1L MoS2 in contact with Au. Nanoscale resolution current mapping and current-voltage (I-V) measurements by conductive atomic force microscopy (C-AFM) showed direct tunneling across the 1L MoS2 on Au, with a broad distribution of tunneling barrier values (ΦB from 0.7 to 1.7 eV) consistent with p-type doping of MoS2. After the final transfer of 1L MoS2 on Al2O3/Si, the strain was converted to compressive strain (ε ≈ -0.25%). Furthermore, an n-type doping (n ≈ 0.5 × 1013 cm-2) was deduced by Raman mapping and confirmed by electrical measurements of an Al2O3/Si back-gated 1L MoS2 transistor. These results provide a deeper understanding of the Au-assisted exfoliation mechanism and can contribute to its widespread application for the realization of novel devices and artificial vdW heterostructures.

A Comparative Study of Top-Down and Bottom-Up Carbon Nanodots and Their Interaction with Mercury Ions.

We report a study of carbon dots produced via bottom-up and top-down routes, carried out through a multi-technique approach based on steady-state fluorescence and absorption, time-resolved fluorescence spectroscopy, Raman spectroscopy, infrared spectroscopy, and atomic force microscopy. Our study focuses on a side-to-side comparison of the fundamental structural and optical properties of the two families of fluorescent nanoparticles, and on their interaction pathways with mercury ions, which we use as a probe of surface emissive chromophores. Comparison between the two families of carbon dots, and between carbon dots subjected to different functionalization procedures, readily identifies a few key structural and optical properties apparently common to all types of carbon dots, but also highlights some critical differences in the optical response and in the microscopic mechanism responsible of the fluorescence. The results also provide suggestions on the most likely interaction sites of mercury ions at the surface of carbon dots and reveal details on mercury-induced fluorescence quenching that can be practically exploited to optimize sensing applications of carbon dots.

Ultrafast Interface Charge Separation in Carbon Nanodot-Nanotube Hybrids.

Carbon dots are an emerging family of zero-dimensional nanocarbons behaving as tunable light harvesters and photoactivated charge donors. Coupling them to carbon nanotubes, which are well-known electron acceptors with excellent charge transport capabilities, is very promising for several applications. Here, we first devised a route to achieve the stable electrostatic binding of carbon dots to multi- or single-walled carbon nanotubes, as confirmed by several experimental observations. The photoluminescence of carbon dots is strongly quenched when they contact either semiconductive or conductive nanotubes, indicating a strong electronic coupling to both. Theoretical simulations predict a favorable energy level alignment within these complexes, suggesting a photoinduced electron transfer from dots to nanotubes, which is a process of high functional interest. Femtosecond transient absorption confirms indeed an ultrafast (<100 fs) electron transfer independent of nanotubes being conductive or semiconductive in nature, followed by a much slower back electron transfer (≈60 ps) from the nanotube to the carbon dots. The high degree of charge separation and delocalization achieved in these nanohybrids entails significant photocatalytic properties, as we demonstrate by the reduction of silver ions in solution. The results are very promising in view of using these "all-carbon" nanohybrids as efficient light harvesters for applications in artificial photocatalysis and photosynthesis.

Folic acid-functionalized graphene oxide nanosheets via plasma etching as a platform to combine NIR anticancer phototherapy and targeted drug delivery.

PEGylated graphene oxide (GO) has shown potential as NIR converting agent to produce local heat useful in breast cancer therapy, since its suitable photothermal conversion, high stability in physiological fluids, biocompatibility and huge specific surface. GO is an appealing nanomaterial for potential clinical applications combining drug delivery and photothermal therapy in a single nano-device capable of specifically targeting breast cancer cells. However, native GO sheets have large dimensions (0.5-5 µm) such that tumor accumulation after a systemic administration is usually precluded. Herein, we report a step-by-step synthesis of folic acid-functionalized PEGylated GO, henceforth named GO-PEG-Fol, with small size and narrow size distribution (∼30 ±â€¯5 nm), and the ability of efficiently converting NIR light into heat. GO-PEG-Fol consists of a nano-GO sheet, obtained by fragmentation of GO by means of non-equilibrium plasma etching, fully functionalized with folic acid-terminated PEG2000 chains through amidic coupling and azide-alkyne click cycloaddition, which we showed as active targeting agents to selectively recognize breast cancer cells such as MCF7 and MDA-MB-231. The GO-PEG-Fol incorporated a high amount of doxorubicin hydrochloride (Doxo) (>33%) and behaves as NIR-light-activated heater capable of triggering sudden Doxo delivery inside cancer cells and localized hyperthermia, thus provoking efficient breast cancer death. The cytotoxic effect was found to be selective for breast cancer cells, being the IC50 up to 12 times lower than that observed for healthy fibroblasts. This work established plasma etching as a cost-effective strategy to get functionalized nano-GO with a smart combination of properties such as small size, good photothermal efficiency and targeted cytotoxic effect, which make it a promising candidate as photothermal agent for the treatment of breast cancer.

Highly Efficient Electron Transfer in a Carbon Dot-Polyoxometalate Nanohybrid.

Using solar radiation to fuel catalytic processes is often regarded as the solution to our energy needs. However, developing effective photocatalysts that are active under visible light has proven to be difficult, often due to the toxicity, instability, and high cost of suitable catalysts. We engineered a novel photoactive nanomaterial obtained by the spontaneous electrostatic coupling of carbon nanodots with [P2W18O62]6-, a molecular catalyst belonging to the class of polyoxometalates. While the former are used as photosensitizers, the latter was chosen for its ability to catalyze reductive reactions such as dye decomposition and water splitting. We find the electron transfer within the nanohybrid to be so efficient that a charge-separated state is formed within 120 fs from photon absorption. These results are a cornerstone in the engineering of a new class of nanodevices, which are nontoxic, are inexpensive, and can carry out solar-driven catalytic processes.

Dynamic Modification of Fermi Energy in Single-Layer Graphene by Photoinduced Electron Transfer from Carbon Dots.

Graphene (Gr)-a single layer of two-dimensional sp2 carbon atoms-and Carbon Dots (CDs)-a novel class of carbon nanoparticles-are two outstanding nanomaterials, renowned for their peculiar properties: Gr for its excellent charge-transport, and CDs for their impressive emission properties. Such features, coupled with a strong sensitivity to the environment, originate the interest in bringing together these two nanomaterials in order to combine their complementary properties. In this work, the investigation of a solid-phase composite of CDs deposited on Gr is reported. The CD emission efficiency is reduced by the contact of Gr. At the same time, the Raman analysis of Gr demonstrates the increase of Fermi energy when it is in contact with CDs under certain conditions. The interaction between CDs and Gr is modeled in terms of an electron-transfer from photoexcited CDs to Gr, wherein an electron is first transferred from the carbon core to the surface states of CDs, and from there to Gr. There, the accumulated electrons determine a dynamical n-doping effect modulated by photoexcitation. The CD-graphene interaction unveiled herein is a step forward in the understanding of the mutual influence between carbon-based nanomaterials, with potential prospects in light conversion applications.

Study of silica-based intrinsically emitting nanoparticles produced by an excimer laser.

We report an experimental study demonstrating the feasibility to produce both pure and Ge-doped silica nanoparticles (size ranging from tens up to hundreds of nanometers) using nanosecond pulsed KrF laser ablation of bulk glass. In particular, pure silica nanoparticles were produced using a laser pulse energy of 400 mJ on pure silica, whereas Ge-doped nanoparticles were obtained using 33 and 165 mJ per pulse on germanosilicate glass. The difference in the required energy is attributed to the Ge doping, which modifies the optical properties of the silica by facilitating energy absorption processes such as multiphoton absorption or by introducing absorbing point defects. Defect generation in bulk pure silica before nanoparticle production starts is also suggested by our results. Regarding the Ge-doped samples, scanning electron microscopy (SEM) and cathodoluminescence (CL) investigations revealed a good correspondence between the morphology of the generated particles and their emission signal due to the germanium lone pair center (GLPC), regardless of the energy per pulse used for their production. This suggests a reasonable homogeneity of the emission features of the samples. Similarly, energy dispersive X-ray spectroscopy (EDX) data showed that the O, Ge and Si signals qualitatively correspond to the particle morphology, suggesting a generally uniform chemical composition of the Ge-doped samples. No significant CL signal could be detected in pure silica nanoparticles, evidencing the positive impact of Ge for the development of intrinsically emitting nanoparticles. Transmission electron microscope (TEM) data suggested that the Ge-doped silica nanoparticles are amorphous. SEM and TEM data evidenced that the produced nanoparticles tend to be slightly more spherical in shape for a higher energy per pulse. Scanning transmission electron microscope (STEM) data have shown that, regardless of size and applied energy per pulse, in each nanoparticle, some inhomogeneity is present in the form of brighter (i.e., more dense) features of a few nanometers.

Impact of contact resistance on the electrical properties of MoS2 transistors at practical operating temperatures.

Molybdenum disulphide (MoS2) is currently regarded as a promising material for the next generation of electronic and optoelectronic devices. However, several issues need to be addressed to fully exploit its potential for field effect transistor (FET) applications. In this context, the contact resistance, RC, associated with the Schottky barrier between source/drain metals and MoS2 currently represents one of the main limiting factors for suitable device performance. Furthermore, to gain a deeper understanding of MoS2 FETs under practical operating conditions, it is necessary to investigate the temperature dependence of the main electrical parameters, such as the field effect mobility (µ) and the threshold voltage (Vth). This paper reports a detailed electrical characterization of back-gated multilayer MoS2 transistors with Ni source/drain contacts at temperatures from T = 298 to 373 K, i.e., the expected range for transistor operation in circuits/systems, considering heating effects due to inefficient power dissipation. From the analysis of the transfer characteristics (ID-VG) in the subthreshold regime, the Schottky barrier height (ΦB ≈ 0.18 eV) associated with the Ni/MoS2 contact was evaluated. The resulting contact resistance in the on-state (electron accumulation in the channel) was also determined and it was found to increase with T as RC proportional to T3.1. The contribution of RC to the extraction of µ and Vth was evaluated, showing a more than 10% underestimation of µ when the effect of RC is neglected, whereas the effect on Vth is less significant. The temperature dependence of µ and Vth was also investigated. A decrease of µ proportional to 1/Tα with α = 1.4 ± 0.3 was found, indicating scattering by optical phonons as the main limiting mechanism for mobility above room temperature. The value of Vth showed a large negative shift (about 6 V) increasing the temperature from 298 to 373 K, which was explained in terms of electron trapping at MoS2/SiO2 interface states.

Ambipolar MoS2 Transistors by Nanoscale Tailoring of Schottky Barrier Using Oxygen Plasma Functionalization.

One of the main challenges to exploit molybdenum disulfide (MoS2) potentialities for the next-generation complementary metal oxide semiconductor (CMOS) technology is the realization of p-type or ambipolar field-effect transistors (FETs). Hole transport in MoS2 FETs is typically hampered by the high Schottky barrier height (SBH) for holes at source/drain contacts, due to the Fermi level pinning close to the conduction band. In this work, we show that the SBH of multilayer MoS2 surface can be tailored at nanoscale using soft O2 plasma treatments. The morphological, chemical, and electrical modifications of MoS2 surface under different plasma conditions were investigated by several microscopic and spectroscopic characterization techniques, including X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), conductive AFM (CAFM), aberration-corrected scanning transmission electron microscopy (STEM), and electron energy loss spectroscopy (EELS). Nanoscale current-voltage mapping by CAFM showed that the SBH maps can be conveniently tuned starting from a narrow SBH distribution (from 0.2 to 0.3 eV) in the case of pristine MoS2 to a broader distribution (from 0.2 to 0.8 eV) after 600 s O2 plasma treatment, which allows both electron and hole injection. This lateral inhomogeneity in the electrical properties was associated with variations of the incorporated oxygen concentration in the MoS2 multilayer surface, as shown by STEM/EELS analyses and confirmed by ab initio density functional theory (DFT) calculations. Back-gated multilayer MoS2 FETs, fabricated by self-aligned deposition of source/drain contacts in the O2 plasma functionalized areas, exhibit ambipolar current transport with on/off current ratio Ion/Ioff ≈ 103 and field-effect mobilities of 11.5 and 7.2 cm2 V-1 s-1 for electrons and holes, respectively. The electrical behavior of these novel ambipolar devices is discussed in terms of the peculiar current injection mechanisms in the O2 plasma functionalized MoS2 surface.

In-situ monitoring by Raman spectroscopy of the thermal doping of graphene and MoS2 in O2-controlled atmosphere.

The effects of temperature and atmosphere (air and O2) on the doping of monolayers of graphene (Gr) on SiO2 and Si substrates, and on the doping of MoS2 multilayer flakes transferred on the same substrates have been investigated. The investigations were carried out by in situ micro-Raman spectroscopy during thermal treatments up to 430 °C, and by atomic force microscopy (AFM). The spectral positions of the G and 2D Raman bands of Gr undergo only minor changes during treatment, while their amplitude and full width at half maximum (FWHM) vary as a function of the temperature and the used atmosphere. The thermal treatments in oxygen atmosphere show, in addition to a thermal effect, an effect attributable to a p-type doping through oxygen. The thermal broadening of the line shape, found during thermal treatments by in situ Raman measurements, can be related to thermal phonon effects. The absence of a band shift results from the balance between a red shift due to thermal effects and a blue shift induced by doping. This shows the potential of in situ measurements to follow the doping kinetics. The treatment of MoS2 in O2 has evidenced a progressive erosion of the flakes without relevant spectral changes in their central zone during in situ measurements. The formation of MoO3 on the edges of the flakes is observed indicative of the oxygen-activated transformation.