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Composite polymer electrolytes are systems of choice for future solid-state lithium metal batteries (LMBs). Poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) is among the most interesting matrices to develop new generation quasi-solid electrolytes (QSEs). Here it is reported on nanocomposites made of PVDF-HFP and pegylated SiO2 nanoparticles. Silica-based hybrid nanofillers are obtained by grafting chains of poly(ethylene glycol) methyl ether (PEG) with different molecular weight on the surface of silica nanoparticles. The functionalized nanofiller improves the mechanical, transport and electrochemical properties of the QSEs, which show good ionic conductivity values and high resistance against dendrite penetration, ensuring boosted long and safe device operation. The most promising result is obtained by dispersing 5 wt% of SiO2 functionalized with short PEG chains (PEG750, Mw = 750 g mol−1) in the PVDF-HFP matrix with an ease solvent-casting procedure. It shows ionic conductivity of 0.1 mS cm−1 at 25 °C, more than 250 h resistance to stripping/plating, and impressive results during cycling tests in LMB with LiFePO4 cathode.

Fe-Nx-C electrocatalysts for the oxygen reduction reaction are typically fabricated via pyrolysis. However, the pyrolysis process is poorly understood. Therefore, a systematic investigation was initiated to elucidate the effects of the pyrolysis conditions (atmosphere and temperature) on the evolution of active sites starting from iron phthalocyanine supported over carbon black. The atomic level dispersion of Fe-Nx is sustained up to 600 °C and afterward, the growth of iron oxide nanoparticles is observed. Interestingly, the different X-ray absorption spectroscopy fingerprints acquired during in-situ and ex-situ experiments indicated the bonding of oxygen as a fifth ligand on the Fe sites when exposed to the open air. The ORR activities were analyzed in acidic and alkaline media. The best electrocatalytic activity was observed for the electrocatalysts pyrolyzed at 600 °C. Above this temperature, a reduction in the activity was observed. Surface-to-reactivity analysis was carried out identifying the relationship between surface chemistry/morphology and electrocatalytic activity.

A novel route for the valorization of waste into valuable products was developed. Surgical masks commonly used for COVID 19 protection by stopping aerosol and droplets have been widely used, and their disposal is critical and often not properly pursued. This work intended to transform surgical masks into platinum group metal-free electrocatalysts for oxygen reduction reaction (ORR) and hydrogen evolution reaction (HER) as well as into crude oil. Surgical masks were subjected to controlled-temperature and -atmosphere pyrolysis, and the produced char was then converted into electrocatalysts by functionalizing it with metal phthalocyanine of interest. The electrocatalytic performance characterization towards ORR and HER was carried out highlighting promising activity. At different temperatures, condensable oil fractions were acquired and thoroughly analyzed. Transformation of waste surgical masks into electrocatalysts and crude oil can open new routes for the conversion of waste into valuable products within the core of the circular economy.

Making a consistency with the objectives of circular economy, herein, waste pistachios shells were utilized for the development of hydrogen evolution reaction (HER) and oxygen reduction reaction (ORR) electrocatalysts which are the key bottleneck in the technological evolution of electrolyzers and fuel cells, respectively. As an alternative to scarce and expensive platinum-group-metal (PGM) electrocatalysts, metal nitrogen carbons (MNCs) are emerging as a promising candidate for both aforementioned electrocatalysis where iron and nickel are the metal of choice for ORR and HER, respectively. Therefore, FeNCs and NiNCs were fabricated utilizing inedible pistachio shells as a low-cost biosource of carbon. The steps involved in the fabrication of electrocatalyst were correlated with electrochemical performance in alkaline media. Encouraging onset potential of ~ 0.88 V vs RHE with a possibility of a 2 + 2 reaction pathway was observed in pyrolyzed and ball-milled FeNC. However, HF etching for template removal slightly affected the kinetics and eventually resulted in a relatively higher yield of peroxide. In parallel, the pyrolyzed NiNC demonstrated a lower HER overpotential of ~ 0.4 V vs RHE at − 10 mA cm−2. Nevertheless, acid washing adversely affected the HER performance and consequently, very high overpotential was witnessed.

The use of glassceramics in photocatalysis is an attractive option for the realization of smart optical fibers and self-cleaning windows. Here we present the photocatalytic activity of germanosilicate glasses embedding Ga2O3 nanocrystals prepared by batch melting and glass heat treatment. The powdered material is used for UV-assisted degradation of rhodamine in water. The kinetics show changes after repeated experiments. In the first cycle, the apparent rate is governed by a second-order reaction with a Gaussian-like shape, whereas the second cycle follows a first-order reaction. The modification appears to be correlated with perturbations in the defect population. Photoluminescence has been used to monitor the evolution of such defects. Kinetic data on photoreactions and defect formation have been modelled in a combined frame in which the defect concentration determines the photocatalytic activity. The results prove the photocatalytic ability of the studied glassceramics. Moreover, the general validity of the kinetic model can be of interest for other systems in which the photocatalytic response depends on photoreactive species concentration.

We report a study of composite scintillating ceramics based on coupled layers of two different garnets, namely Ce-doped gadolinium gallium aluminium (GGAG:Ce) and Pr-doped yttrium aluminium (YAG:Pr), fabricated by hot isostatic pressing. Two samples were prepared, with different GGAG:Ce layer thickness, 120 µm and 690 µm respectively, but with a comparable overall thickness of 1.4 mm. The key finding is that the material architecture strongly determines the scintillation response. The radioluminescence is that expected from the irradiated material when a thick layer of ceramic is exposed to X-rays. Conversely, exposing a thin layer allows a non-null probability —about 0.3% for 120 µm of GGAG— of finding an X-ray photon in the underlying layer, and thus radioluminescence from both materials is recorded. We believe these results can extend the potential of layered optical ceramics for advanced devices, such as energy- and direction-sensitive X-ray detectors.

Metal-nitrogen-carbons (M-N-Cs) as a reliable substitution for platinum-group-metals (PGMs) for oxygen reduction reaction (ORR) are emerging candidates to rationalize the technology of fuel cells. The development of M-N-Cs can further be economized by consuming waste biomass as an inexpensive carbon source for the electrocatalyst support. Herein, we report the simple fabrication and in-depth characterization of electrocatalysts using lignin-derived activated char. The activated char (LAC) was functionalized with metal phthalocyanine (FePc and MnPc) via atmosphere-controlled pyrolysis to produce monometallic M-N-Cs (L_Mn and L_Fe) and bimetallic M1-M2-N-Cs (L_FeMn) electrocatalysts. Raman spectroscopy and transmission electron microscopy (TEM) revealed a defect-rich architecture. XPS confirmed the coexistence of various nitrogen-containing active moieties. L_Fe and L_FeMn demonstrated appreciable ORR in both acidic and alkaline conditions whereas L_FeMn helped in restricting the peroxide yield, particularly in alkaline media. L_Fe and L_FeMn demonstrated remarkable onset potential (Eonset) of ∼0.942 V (vs RHE) with an E1/2 of 0.874 V (vs RHE) in 0.1 M KOH. In acid, L_FeMn had an Eonset of 0.817 V (vs RHE) and an E1/2 of ∼0.76 V (vs RHE). Finally, the L_FeMn as a cathode electrocatalyst was integrated and tested in PEMFC and AEMFC. AEMFC demonstrated optimistic performance with a peak power density of 261 mW cm−2 at the current density of ∼577 mA cm−2.

Among the materials for the negative electrodes in Li-ion batteries, oxides capable of reacting with Li+ via intercalation/conversion/alloying are extremely interesting due to their high specific capacities but suffer from poor mechanical stability. A new way to design nanocomposites based on the (Ti/Sn)O2 system is the partial oxidation of the tin-containing MAX phase of Ti3Al(1-x)SnxO2 composition. Exploiting this strategy, this work develops composite electrodes of (Ti/Sn)O2 and MAX phase capable of withstanding over 600 cycles in half cells with charge efficiencies higher than 99.5% and specific capacities comparable to those of graphite and higher than lithium titanate (Li4Ti5O12) or MXenes electrodes. These unprecedented electrochemical performances are also demonstrated at full cell level in the presence of a low cobalt content layered oxide and explained through an accurate chemical, morphological, and structural investigation which reveals the intimate contact between the MAX phase and the oxide particles. During the oxidation process, electroactive nanoparticles of TiO2 and Ti(1-y)SnyO2 nucleate on the surface of the unreacted MAX phase which therefore acts both as a conductive agent and as a buffer to preserve the mechanical integrity of the oxide during the lithiation and delithiation cycles.

Exposure of polymers to ionizing radiation and high-energy particle beams is involved in many processes – from food sterilization to radiotherapy protocols. The resulting effects, at the final stages, determine the functional, structural, and morphological alteration of the material. However, the processes responsible for cumulative chain scission, crosslinking, and reactions with the environment are often difficult to disentangle as a sequence of elementary events. Here we report a spectroscopic study – by attenuated-total reflection Fourier transform infrared spectroscopy and powder x-ray diffraction measurements, together with differential scanning calorimetry and thermogravimetric analyses – that sheds light on the very initial stages of the mechanisms involved in radiation-induced modifications of poly(lactic acid) (PLA). The results, collected on samples from biobased processes and exposed to low x-ray doses in the range of 100–103Gy after different thermal treatments, show spectroscopic evidence of the emergence of molecular unit perturbations – mainly related to methyl and carbonyl groups with the formation of C=C double bonds – with a clear-cut dependence on the polymer conformation. Understanding the mechanisms involved and the role of crystallinity provides information potentially useful for the development of PLA with a suitable radiation hardness for applications in radiotherapy.

Highly concentrated aqueous binary solutions of acetate salts are promising systems for different electrochemical applications, for example, energy storage devices. The very high solubility of CH3COOK allows us to obtain water-in-salt electrolyte concentrations, thus reducing ion activity and extending the cathodic stability of an aqueous electrolyte. At the same time, the presence of Li+ or Na+ makes these solutions compatible with intercalation materials for the development of rechargeable alkaline-ion batteries. Although there is a growing interest in these systems, a fundamental understanding of their physicochemical properties is still lacking. Here, we report and discuss the physicochemical and electrochemical properties of a series of solutions based on 20 mol kg-1 CH3COOK with different concentrations of CH3COONa. The most concentrated solution, 20 mol kg-1 CH3COOK + 7 mol kg-1 CH3COONa, gives the best compromise between transport properties and electrochemical stability, displaying a conductivity of 21.2 mS cm-1 at 25 °C and a stability window of up to 3 V in “ideal” conditions, i.e., using a small surface area and highly electrocatalytic electrode in a flooded cell. Careful Raman spectroscopy analyses help to address the interaction network, the phase evolution with temperature, and the crystallization kinetics.

Self-assembly peptides (SAPs) are an important class of hydrogels used in nanomedicine for tissue repair and neural regeneration. Due to their unique properties, SAPs may be used in a wide range of applications but some limitations, such as low bioavailability and rapid hydrolysis degradation, need to be overcome. Here, we describe the synthesis and characterization of two novel cyclic SAPs without the use of D/L-alternating amino acids, showing a reversible transition of their supramolecular nanostructures, from nanotubes/nanofibers into nanovesicles/nanospheres. The investigation, characterization and optimization are performed using atomic force microscopy (AFM), attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, Raman analysis, circular dichroism (CD), and rheology measurements. Also, in vitro cell viability assays show negligible toxicity of the representative optimized cyclic SAP towards human neural stem cells (hNSCs). Our results suggest that linear SAP theoretical background can be applied to develop cyclic SAPs, with important implications in the scalable fabrication of inter-changeable nanostructures, as well as for biomedical applications, including tissue regeneration, drug-delivery, drug-design, sensing, imaging, and size selectivity.

Many efforts are currently focused on materials with responsive features for neural-inspired devices. Different approaches are followed, based on various mechanisms – from ferroelectric switching to structural phase changes, from magnetic tunnel junctions to metal filament formation. Here we analyze an alternative strategy based on an unconventional electrical response arising from percolative charge transport and charge trapping in discrete random networks of oxide nanostructures in a dielectric matrix. After an analysis of the mechanisms which can potentially be a source of a plastic response in this class of systems, we report evidence of this behavior in a system comprising an alkali-germanosilicate amorphous matrix with incorporated Ga-oxide nanostructures. The active material – consisting in a film 70 nm thick interfaced to p-type Si and Au electrodes – gives a responsive behavior to pulsed bias which is accompanied by bias dependent electric conduction, with resistivity changes of an order of magnitude by applying 2 V, as well as a dielectric response with hysteretic features, as expected by the model. The results represent a first proof of concept of an unexplored strategy for the design of responsive systems.

Within the framework of the circular economy, the waste litchi's skins were upgraded and transformed into electrocatalysts for oxygen reduction reaction (ORR) and hydrogen evolution reaction (HER). The waste litchi's skins were pyrolyzed, activated, and then used as carbon support for fabricating metal–nitrogen–carbons (M–N–Cs) which belong to a promising class of platinum group metal-free electrocatalysts. The activated char was functionalized with transition metal (Fe, Ni, and Co)- phthalocyanine (Pc) in monometallic and bimetallic fashion by subjecting it to a thermal treatment at 600 and 900°C. The samples functionalized at 900°C showed higher performance for HER due to the formation of metal nanoparticles, whereas the samples functionalized at 600°C showed higher performance for ORR. Particularly, sample Ni–Co 900 had an overpotential of −0.38 V for HER, while the sample Fe 600 was the most active electrocatalyst for ORR by demonstrating the onset potential of ∼0.9 V (a half-wave potential of ∼0.81 V) with the least production of unwanted peroxide anion.

Following the core theme of a circular economy, a novel strategy to upcycle cigarette butt waste into platinum group metal (PGM)-free metal nitrogen carbon (M-N-C) electrocatalysts for oxygen reduction reaction (ORR) is presented. The experimental route was composed of (i) the transformation of the powdered cigarette butts into carbonaceous char via pyrolysis at 450 °C, 600 °C, 750 °C and 900 °C, (ii) the porosity activation with KOH and (iii) the functionalization of the activated chars with iron (II) phthalocyanine (FePc). The electrochemical outcomes obtained by the rotating disk electrode (RRDE) technique revealed that the sample pyrolyzed at 450 °C (i.e., cig_450) outperformed the other counterparts with its highest onset (Eon) and half-wave potentials (E1/2) and demonstrated nearly tetra-electronic ORR in acidic, neutral and alkaline electrolytes, all resulting from the optimal surface chemistry and textural properties.

We present a completely non-destructive approach to analyse a set of historical glass mosaic tesserae. Aim of the study is to obtain a qualitative and quantitative characterization of the glass matrix in terms of elements and mineralogical phases. Several non-destructive techniques have been applied like Particle-Induced X-ray Emission, Particle-Induced Gamma-ray Emission, micro-Raman spectroscopy, neutron resonance capture analysis and neutron activation analysis in order to combine different technique strengths and to explore the effect of different range sizes for the analysis. Yet, best practices require the use of combined analysis and different skills. The paradigm of a non-destructive multi-analytical approach is suggested for a comprehensive investigation in non-homogeneous real samples, like historical glass mosaic tesserae.

The influence of Al2O3 as an additive and the heat-treatment regime on the luminescence spectra of gallate glass-ceramics was investigated. It is shown that its luminescence efficiency can be enhanced by changing the submicron-inhomogeneous structure of the initial glasses.

Water-in-salt solutions, i.e. solutions in which the amount of salt by volume or weight is larger than that of the solvent, are attracting increasing attention in electrochemistry due to their distinct features that often include decomposition potentials much higher than those of lower concentration solutions. Despite the high solubility of potassium acetate (KAC) in water at room temperature (up to 25 moles of salt per kg of solvent), the low cost, and the large availability, the use of highly concentrated KAC solutions is still limited to a few examples in energy storage applications and a systematic study of their physical-chemical properties is lacking. To fill this gap, we have investigated the thermal, rheological, electrical, electrochemical, and spectroscopic features of KAC/water solutions in the compositional range between 1 and 25 mol kg-1. We show the presence of a transition between the "salt-in-solvent"and "solvent-in-salt"regimes in the range of 10-15 mol kg-1. Among the explored compositions, the highest concentrations (20 and 25 mol kg-1) exhibit good room temperature conductivity values (55.6 and 31 mS cm-1, respectively) and a large electrochemical potential window (above 2.5 V).

The influence of fiber drawing on mechanical and vibrational properties of RE-doped sol-gel silica is disclosed by a comparison of bulk silica, before and after the melting process, and fibers. The mechanical characterization is carried out by nanoindentation technique: hardness and elastic modulus are found to be consistent with those of Corning 7980 reference glass, and related to the elasto-plastic behavior of the glassy material. Our results evidence an increase of the resistance of fibers to fracture under an applied load, ascribed to drawing-induced residual stresses. Their impact on sol-gel silica mechanical properties is further disclosed by complementary vibrational characterization by Raman and FTIR spectroscopies, confirming the occurrence of a modification of the structural features after the drawing process and of residual stresses in the fibers. The overall results highlight the role of the fiber drawing in improving the glass mechanical properties, causing a slight rearrangement of the silica structure.

Water in salt solutions are a new class of electrolytes developed with the aim of increasing the electrochemical stability of aqueous electrolytes without decreasing the transport properties. Among them, aqueous solutions of potassium acetate (CH3COOK, AcK) have received little attention, despite its large solubility in water at room temperature (25 mol kg−1) and the very low cost. With the idea of developing cost-effective and good performing Electrochemical Double Layer Capacitors (EDLCs), a symmetric device based on a low-cost coal derived carbon (F400) and highly concentrated AcK solutions as electrodes and electrolytes, respectively, was fabricated and optimized. The best results are obtained with the system F400/20 mol kg−1 AcK/F400 able to deliver a gravimetric energy density of 26 Wh kg−1 at an average power of 1.4 kW kg−1.

Tailoring the precise construction of non-precious metals and carbon-based heterogeneous catalysts for electrochemical oxygen evolution reaction (OER) and methanol oxidation reaction (MOR) is crucial for energy conversion applications. Herein, this work reports the composite of Ni doped Fe2 O3 (Ni-Fe2 O3 ) with mildly oxidized multi-walled CNT (O-CNT) as an outstanding Mott-Schottky catalyst for OER and MOR. O-CNT acts as a co-catalyst which effectively regulates the charge transfer in Ni-Fe2 O3 and thus enhances the electrocatalytic performance. Ni-Fe2 O3 /O-CNT exhibits a low onset potential of 260 mV and overpotential 310 mV @ 10 mA cm-2 for oxygen evolution. Being a Mott-Schottky catalyst, it achieves the higher flat band potential of -1.15 V with the carrier density of 0.173×1024 cm-3 . Further, in presence of 1 M CH3 OH, it delivers the MOR current density of 10 mA cm-2 at 1.46 V vs. RHE. The excellent electrocatalytic OER and MOR activity of Ni-Fe2 O3 /O-CNT could be attributed to the synergistic interaction between Ni-doped Fe2 O3 and O-CNT.

In this study, we report the experimental findings of a multi-methodological and comparative investigation of a natural (from the Wah Wah Mountains of Beaver County, Utah) and three synthetic (hydrothermally grown) gem-quality red beryls by means of: gemmological standard testing, laser ablation inductively coupled mass spectroscopy, infrared and Raman spectroscopy, ultraviolet–visible–near infrared absorption spectroscopy, and single-crystal X-ray diffraction. Gemmological, crystallo-chemical, and spectroscopic features of the natural and synthetic stones enabled us to unveil the causes of their color (from red, to purplish-red, or orange-red) and how different and complementary techniques can be efficiently used to discriminate between natural and synthetic materials, based on non-destructive, micro-destructive, and destructive techniques.

Agates from Yozgat province are appreciated on the gem market for their white and purple-blue banded colours. In this study, we present a detailed investigation aimed at the identification of the atomic and structural origin of this peculiar colouration of chalcedony. X-ray diffraction and Raman spectroscopy revealed the presence of fine grains of quartz and moganite with a preferential accumulation of the latter in the blue bands. Near-infrared diffuse absorption spectra show overtones of hydroxyls vibrations at 1425, 1900, and 2250 nm. In the visible, the broad absorption at about 500 nm, as well as its behaviour at low temperatures, is compatible with the optical activity of iron impurities in quartz matrices, such as that observed in amethysts. Peak intensities and shapes are very similar for spectra collected in blue and white bands. Accordingly, trace-element composition from laser ablation inductively coupled mass spectrometry confirmed that the two regions have similar Fe content. The perceived changes in band colours are indeed originated by differences in microstructural arrangement and size of the grains visualised through scanning electron microscopy. White and blue stripes have grains of about 5 µm and 300 nm in size, respectively, resulting in an accentuated scattering component for the white bands. Therefore, the unique purple-blue shades typical of Yozgat agates are a combination of iron-related colour centres and scattering effect.

The development of hybrid nanoscintillators is hunted for the implementation of modern detection technologies, like in high energy physics, homeland security, radioactive gas sensing, and medical imaging, as well as of the established therapies in radiation oncology, such as in X-ray activated photodynamic therapy. Engineering of the physico-chemical properties of nanoparticles (NPs) enables the manufacture of hybrids in which the conjugation of inorganic/organic components leads to increased multifunctionality and performance. However, the optimization of the properties of nanoparticles in combination with the use of ionizing radiation is not trivial: a complete knowledge on the structure, composition, physico-chemical features, and scintillation property relationships in hybrid nanomaterials is pivotal for any applications exploiting X-rays. In this paper, the design of hybrid nanoscintillators based on ZnO grown onto porous SiO2 substrates (ZnO/SiO2) has been performed in the view to create nanosystems potentially suitable in X-ray activated photodynamic therapy. Indeed, cytotoxic porphyrin dyes with increasing concentrations have been anchored on ZnO/SiO2 nanoparticles through amino-silane moieties. Chemical and structural analyses correlated with photoluminescence reveal that radiative energy transfer between ZnO and porphyrins is the principal mechanism prompting the excitation of photosensitizers. The use of soft X-ray excitation results in a further sensitization of the porphyrin emission, due to augmented energy deposition promoted by ZnO in the surroundings of the chemically bound porphyrin. This finding unveils the cruciality of the design of hybrid nanoparticles in ruling the efficacy of the interaction between ionizing radiation and inorganic/organic moieties, and thus of the final nanomaterial performances towards the foreseen application.

Mass generation of scrap tires presents a major challenge for environmental safety, however, their upcycling into carbon-based nanomaterials by the virtue of pyrolysis treatments can open up new windows for energy conversion and storage technologies in the context of the circular economy. Herein, we report the synthesis of Fe-N-C oxygen reduction reaction (ORR) electrocatalyst for fuel cell (FC) applications using carbonaceous char derived from scrap tires through microwave-assisted pyrolysis (MAP). The char obtained from MAP was activated with potassium hydroxide and then pyrolyzed at a high temperature to fabricate Fe-N-C after mixing with iron and nitrogen precursors. Finally, the developed Fe-N-C was ball-milled and acid-etched for homogenization and leaching of iron oxide nanoparticles. In this study, structural evaluation during each synthesis step was elucidated and correlated with the ORR activity in all three pHs i.e. acidic, neutral, and alkaline. Moreover, the effect of electrocatalyst loading on ORR kinetics was also analyzed using two different loadings (0.2 and 0.6 mg cm−2) on the rotating ring disk electrode (RRDE). The developed Fe-N-C demonstrated encouraging onset potentials of 0.881, 0.822, and 0.936 V vs RHE in acidic, neutral, and alkaline conditions, respectively. Whereas the ORR activity was slightly reduced after the milling-etching step. Lower peroxide yield together with a tetra-electronic reduction of oxygen was witnessed in acidic and neutral conditions, however, peroxide production was increased in the alkaline medium.

Lithium metal batteries (LMBs) will be a breakthrough in automotive applications, but they require the development of next-generation solid-state electrolytes (SSEs) to stabilize the anode interface. Polymer-in-ceramic PEO/TiO2 nanocomposite SSEs show outstanding properties, allowing unprecedented LMBs durability and self-healing capabilities. However, the mechanism underlying the inhibition/delay of dendrite growth is not well understood. In fact, the inorganic phase could act as both a chemical and a mechanical barrier to dendrite propagation. Combining advanced in situ and ex situ experimental techniques, we demonstrate that oligo(ethylene oxide)-capped TiO2, although chemically inert toward lithium metal, imparts SSE with mechanical and dynamical properties particularly favorable for application. The self-healing characteristics are due to the interplay between mechanical robustness and high local polymer mobility which promotes the disruption of the electric continuity of the lithium dendrites (razor effect).

Ionic liquids (ILs) are an increasingly important component of electrolytes for lithium and sodium batteries. Here, the physicochemical properties of the system N-propyl-N-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide (Pyr13TFSI) ionic liquid and NaTFSI are investigated vs. the concentration of the sodium salt and the temperature. The explored concentration range was (1-x) Pyr13TFSI: x NaTFSI with x (mole fraction) = 0, 0.02, 0.05, 0.1, 0.2. 23Na solid-state NMR reveals that the Na+ ions exist in two distinct environments: mobile Na+ ions (1), and Na+ ions involved in clusters or even bigger interacting networks (2). The ratio between mobile and bonded Na+ populations increases with temperature and decreases with increasing salt concentration, reaching 100% at 60 °C for the most diluted compositions. Raman spectroscopy allows to identify the quantity of free and bonded anions depending on the concentration, and to measure the number of Na+ ions solvating the TFSI− anion (SN = 4). The combined NMR and Raman results allow us to estimate the salt solubility range, x = 0.12 ± 0.02. The composition x = 0.1 showed satisfying stability when cycled versus high-potential cathodic material Na0.44MnO2 (NMO) in a cell Na/IL/NMO.