The purpose of this paper is to present a summary of the application of non-destructive tech- niques used in a comparative study of eighty pottery fragments of the Chalcolithic period (5000 BC ca.) and Late Bronze Age (1650 - 1200 BC ca.), found in Mersin-Yumuktepe (Southern Turkey) and Arslantepe (Malatya, Eastern Turkey)

Aligned selenium microtubes array vertically grown on a silicon substrate was synthesized in a tubular furnace under argon flow at an evaporation temperature of 300 C. The microtubes were characterized byRaman spectroscopy, X-ray diffraction, UV–vis spectroscopy, scanning and transmission electron microscopy. The photoelectrical properties of the microtube array with light were investigated. It was found a stable relative increase of the conductivity by 180% when the sample was taken from the dark and exposed with tungsten light and a sharp on/off switching behavior. These results hold promise for the fabrication of microtubes-detector arrays

An alkoxy-substituted poly(phenylene thiophene) is used in order to suspend single-walled carbon nanotubes in an organic solvent. The suspension is spread on the air–water interface of a Langmuir trough and the floating film is characterized by means of Brewster angle microscopy and UV-visible reflection spectroscopy and the compression isotherm is recorded. The polymer/carbon-nanotube blend is transferred onto different substrates using the Langmuir–Blodgett technique. AFM measurements indicate the formation of globular structures for the samples transferred at low surface-pressure values and a tubular morphology for high-pressure-deposited samples. AFM analysis is repeated on a sample exposed to soft X-rays for about 5 h and a highly organized structure of bundles of carbon nanotubes rises up. Samples with different numbers of layers are transferred onto ITO substrates by means of the Langmuir–Blodgett method and are tested as photocathodes in a photo-electrochemical cell. A Voc of 0.18 V, an Isc of 85.8mA, FF of 40.0%, and h of (6.23T103 )% are obtained.

Iris è una pianta appartenente alla famiglia delle Iridacee, comunemente nota come Giaggiolo o Iris. Al fine di osservare delle differenze tra la struttura riproduttiva e per avanzare delle ipotesi circa la sterilità di molte specie di Iris, è stata condotta l'analisi del polline mediante microscopia elettronica a scansione (SEM). L'analisi micromorfologica dell'esina è utile per identificare probabili formazioni anomale del polline, al fine di preservare le differenti specie e valutare i possibili cambiamenti negli bridi naturali. Lo studio della struttra dell'esina è un importante metodo per classificare differenti specie di Iris, ma anche per dare informazioni circa la formazione del polline. I risultati ottenuti non hanno mostrato anomalie significative tra le differenti specie di Iris analizzate

In this work, we report about the synthesis of silver–titanium dioxide nanostructures and their usage for building up thin films. We shows that nanoparticles of titania enveloped by very thin silver layer were obtained. In addition, these particles were suitable to obtain an active layer for solid-state gas sensor. In particular, we investigate the electrical modifications following the exposure to reactive gases of obtained films. In this way, the sensing performances of active layers were evaluated. The whole sensing characterization was carried out on thin films deposited on alumina and completely processed by microelectronic standard procedures.

A simple and rapid vapor deposition route has been developed for the growth of trigonal phase selenium microtubes in a horizontal tubular furnace under argon flow gas. Selenium powder was evaporated by heating at 300 C, and the vapors were condensed on different quartz substrates located at 70-140 C. It was found that the morphologies of the products were strongly affected by small variations of the temperatures of the deposition zones. It was observed that the growth of microtubes was initiated by formation of nearly spherical microparticles with smooth surfaces; the smooth microspheres were first covered by a rough layer and then they slowly became empty. The additional selenium atoms transported from the heated part of the furnace or coming from the consumption of the inner core of the rough microparticles continued to adsorb on the empty microspheres, allowing two possible growth mechanisms. If the additional Se atoms preferentially went to the circumferential edges of the empty microspheres, crystalline microtubes with no defects were formed; however, Se atoms could also follow a spiral growth mechanism starting from the empty shells. This second growth mechanism led to the formation of semiclosed tubular structures with irregular surfaces, which developed into the relatively completed uniform microtubes with smooth surfaces. The morphology, microstructure, and chemical composition of the microtubes were characterized by various means (X-ray diffraction, energy-dispersive X-ray spectroscopy, Raman spectroscopy,UV-vis spectroscopy, scanning electron microscopy, and transmission electron microscopy). The as-grown Se microtubes may find application as rapid response photosensors and photocells.

Silver nanoparticles were synthesized in the presence of saccharides and ammonia (NH3) in the concentration range from 10−2 to 103 ppm to develop an optical sensor for NH3 in aqueous solutions. Ammonia affects the features of the nanoparticles obtained in a concentration-dependent manner as determined by UV–vis absorption analysis and TEM observations. Structural and morphological analysis provides the basis for the production of a colorimetric label-free sensor for ammonia. Overall, surface plasmon resonance increases when ammonia concentration rises, although the functional trend is not the same over the entire investigated ammonia concentration range. Three different ranges have been identified: very low ammonia concentrations from 0.01 to 0.2 ppm, high ammonia concentrations from 20 to 350 ppm and, most importantly, the intermediate or physiological range of ammonia from 0.5 to 10 ppm.

In this study, monodispersed silver nanoparticles with diameter in the range 4-10 nm were first synthesized by chemical reduction from silver nitrate using glucose as reducing agent and sucralose as capping agent, through microwave assisted method. Then, a strong enhancement of the yield of the synthesized nanoparticles and their self-assembly could be achieved through the injection into the colloidal solution, at room temperature, of a tertiary amine (triethylamine, TEA), which acted both as promoter and as directing agent for silver nanoparticles. The yield of the synthesized nanoparticles and the length of the chains could be tuned by facile adjustment of the TEA concentration and reaction time. The interaction between amine and silver nanoparticles made the non-uniform spatial distribution of stabilizers at nanoparticles surfaces and led to the 1D assembly. Transmission electron microscopy (TEM) and UV-Vis spectroscopy have been employed for monitoring the nanochains formation. This mechanism evidenced that sucralose capped silver nanoparticles could also be useful for the real-time naked-eye detection of amine.

CONTENTS 1. Electron Diffraction: The Beginning of the History 2. ED Techniques Today: A General Overview 3. Application of ED Technique to Carbon-Based Nanomaterials References

We have performed a detailed investigation of the basic electronic transport properties of single walled carbon nanotubes (SWCNT) organized in macroscopic ribbons (some millimeters long with a transversal size of tens of microns), and formed predominantly by identical nanotubes. High resolution TEM and Electron diffraction techniques have been applied in order to determine the peculiar aggregation of SWCNTs in homotype bundles.The electronic properties of individual SWCNT bundles have been investigated by scanning tunneling microscopy and spectroscopy (STM/STS). The electrical features of the ribbons have been investigated in the 100–500 K temperature range using a multifinger device. Overall, the results indicate the possibility to control the local density of state energy by tailoring different architectures.

The development of biocompatible collagen substrates able to conduct electric current along specific pathways represent an appealing issue in tissue engineering, since it is well known that electrical stimuli significantly affects important cell behaviour, such as proliferation, differentiation, directional migration, and, therefore, tissue regeneration. In this work, a cheap and easy approach was proposed to produce collagen-based films exhibiting enhanced electrical conductivity, through the simple manipulation of a weak external magnetic trigger. Paramagnetic iron oxide nanoparticles (NPs) capped by a biocompatible polyethylene-glycol coating were synthetized by a co-precipitation and solvothermic method and sprayed onto a collagen suspension. The system was then subjected to a static external magnetic field in order to conveniently tune NPs organization. Under the action of the external stimulus, NPs were induced to orient along the magnetic field lines, forming long-range aligned micropatterns within the collagen matrix. Drying of the substrate following water evaporation permanently blocked the magnetic architecture produced, thereby preserving NPs organization even after magnetic field removal. Electrical conductivity measurements clearly showed that the presence of such a magnetic framework endowed collagen with marked conductive properties in specific directions. The biocompatibility of the paramagnetic collagen films was also demonstrated by MTT cell cytotoxicity test.

In this study, a fast colorimetric triethylamine sensor based on localized surface plasmon resonance of silver nanoparticles is presented. The nanoparticles were synthesized by chemical reduction from silver nitrate using glucose as reducing agent and sucralose as capping agent.

We present a totally green approach toward the rapid synthesis and stabilization of metal nanoparticles through the treatment of aqueous solutions of silver nitrate with two commonly available sugars, i.e., maltose and sucrose as reducing agents. The average size, size distribution, morphology and internal crystalline structure of the nanoparticles are studied through high resolution transmission electron microscopy, selected-area diffraction pattern and UV–Vis spectroscopic technique and are seen to be critically dependent on the used sugar. The great majority of sucrose-assisted synthesized nanoparticles is distributed in a size range less than 6.0 nm, with an arithmetic media of 5.2 nm and a statistical standard deviation of 1.3 nm. For the maltose synthesized sample, the size distribution plot reveals that nanoparticles are greater (with a mean size of 62.4 nm and a standard deviation of 9.5 nm) and exhibit a more anisotropic morphology.

A surprising and unexpected biomineralization process was observed during toxicological assessment of carbon nanoparticles on Paracentrotus lividus (sea urchin) pluteus larvae. The larvae activate a process of defense against external material, by incorporating the nanoparticles into microstructures of aragonite similarly to pearl oysters. Aiming at a better understanding of this phenomenon, the larvae were exposed to increasing concentrations of carbon nanoparticles and the biomineralization products were analyzed by electron microscopy, x-ray diffraction and Raman spectroscopy. In order to evaluate the possible influence of Sp-CyP-1 expression on this biomineralization process by larvae, analyses of gene expression (Sp-CyP-1) and calcein labeling were performed. Overall, we report experimental evidence about the capability of carbon nanoparticles to induce an increment of Sp-CyP-1 expression with the consequent activation of a biomineralization process leading to the production of a new pearl-like biomaterial never previously observed in sea urchins.

Polymeric and hybrid aqueous-core nanocapsules were prepared using a low energy organic-solvent free procedure as innovative nanodevices for the ophthalmic delivery of melatonin. In order to evaluate how different cationic lipids could affect the main properties of the nanodevices, we focused our attention on mean particles size, surface charge, shape and stability (the "4S"). The results of our study confirmed the hypothesis that the coating material differently affects the overall nanoparticles properties, above all in terms of morphology: in particular, the cationic lipid dimethyldioctadecylammonium bromide allows the formation of very stable well-defined nanocapsules with non-spherical shape with sustained and prolonged drug release, thus representing a great advantage in ophthalmic application.

In this work, we performed experiments of absorption of hydrogen and deuteriumgas by Pd thin films, and we compared the behavior of these samples to unprocessed films. We also employed a continuous wave He–Ne laser to irradiate the samples inside the chamber during the treatment, in order to increase the gas absorption. Using a scanning electron microscope (SEM) and an electron probe micro-analyzer (EDX), we observed structures like spots on the surface of the treated samples. Inside the spots, elements other than Pd were found. Based on these results, we determined that gas loading is an effective way to transmute elements, and the laser action has been a very effective way to increase morphological changes in the treated samples.

Surface-enhanced Raman spectroscopy (SERS) allows a new insight into the analysis of cell physiology. In this work, the difficulty of producing suitable substrates that, besides permitting the amplification of the Raman signal, do not interact with the biological material causing alteration, has been overcome by a combined method of hydrothermal green synthesis and thermal annealing. The SERS analysis of the cell membrane has been performed with special attention to the cellular prion protein PrPC. In addition, SERS has also been used to reveal the prion protein–Cu(II) interaction in four different cell models (B104, SH-SY5Y, GN11, HeLa). A significant implication of the current work consists of the intriguing possibility of revealing and quantifying prion protein expression in complex biological samples by a cheap SERS-based method, replacing the expensive and time-consuming immuno-assay systems commonly employed.

We report about the nanoclustering induced by oxygen‐implantation in silicon. A tandem‐type accelerator, with a maximum acceleration voltage of 3 MV, equipped with a sputtering ion source suitable for the production of high current ion beams by sputtering of solid cathodes has been used. The surface modifications and the structure of nanoclusters are investigated. The topographic images, obtained by scanning tunnelling microscope showed that the surface is covered with a dense array of tetragonal nanostructures oriented with respect to the substrate. Raman spectroscopy data allowed us to estimate an average cluster size of about 50 nm. Resistivity and all effect measurements evidenced that the electron transport in the implanted silicon samples is affected by the nanoclusters array and it could be explained by thermally activated hopping between localized states.

Carbon based nanostructures are interesting building blocks to realize films for a lot of applications that include bio- and chemical-sensing. In this work we present a one-step electrochemical method to produce water-based stable nanographite colloid used to realize lined-up micro-patterned films. The high surfaceto- volume ratio makes these structures suitable for adsorbing gases. Morphological, compositional and structural characterization have been performed in order to determine the features of the films. Simple resistive nanographite devices were fabricated and tested for NO2 sensitivity. Moreover, the present approach represents a general and facile method of good potential for scale-up that could be extended to other materials.

This work enters in an interdisciplinary research project involving the archaeometrical analysis of ancient silver coins minted in the Greek colony of Taras (the modern south Italian town of Taranto) between the V century BC and the III century BC. In this work, by comparing the results obtained from X-ray microanalysis data acquired from the least corroded surface areas and the cross- section of coins from SEM-EDX and from XRF analysis, we have demonstrated that analysed coins exhibited a corrosion layer no more than 25 m and that surface silver enrichment was less than 1 wt%. Thus, the data obtained by using X-ray microanalysis from surface may not significantly differ from the original bulk composition. Our results demonstrate that the silver content in the coins decreases considerably ranging from about 97% for the older down to 80% for the ones of 3rd Evans period (300–270 BC), corresponding to the significant social change in the period.

A supramolecular adduct formed by the interaction among octadecylamine (ODA) and zinc oxide nanostructures was promoted. A stable dispersion of the ZnO@ODA adduct was obtained and characterized by means of thermogravimetric analysis and infrared and Raman spectroscopy. Then, the supramolecular adduct was spread at the air/water interface of a Langmuir trough. The presence of octadecylamine gave amphiphilic features to the ZnO@ODA adduct that was transferred from the air/water interface to solid substrates by Langmuir-Schaefer (LS) method. The transferred film was characterized by tunnel electron microscopy that highlighted rectangular well-shaped structures assembled by nanostructure of ZnO arranged in an ODA matrix. Piezoelectric feature of large LS film (1 cm2) was tested and a very promising response was observed as a consequence of the application of a pressure of 1 kPa.

CTR1 (Copper Transporter 1), PrPC (Cellular Prion Protein), NRAMP2 (Natural Resistance - Associated Macrophage Protein 2) and ATP7A proteins control the cell absorption and efflux of copper (Cu) ions in nervous tissues upon physiological conditions. Little is known about their regulation under reduced Cu availability, a condition underlying the onset of diffused neurodegenerative disorders. In the current study, rat neuron-like cells were exposed to Cu starvation for 48 h. The activation of Caspase-3 enzymes and the impairment of Cu,Zn Superoxide Dismutase (Cu,Zn SOD) activity depicted the initiation of a pro-apoptotic program, preliminary to the appearance of the morphological signs of apoptosis. The transcriptional response related to Cu transport proteins has been investigated. Notably, PrPC transcript and protein levels were consistently elevated upon Cu deficiency. The CTR1 protein amount was stable, despite a two-fold increase in the transcript amount, meaning the activation of post-translational regulatory mechanisms. NRAMP2 and ATP7A expression was unvaried. The up-regulated PrPC has been demonstrated to enhance the cell Cu uptake ability by about 50% with respect to the basal transport, and so sustain the Cu delivery to the Cu,Zn SOD cuproenzymes. Conclusively, the study suggests a pivotal role for PrPC in the cell adaptation to Cu limitation through a direct activity of ion uptake. In this view, the PrPC accumulation observed in several cancer cell lines could be interpreted as a molecular marker of cell Cu deficiency and a potential target of therapeutic interventions against disorders caused by metal imbalances.

The prion proteins and their interaction with copper ion represent a suitable marker in neurodegenerative disorders. A SERS based optical sensor has been developed in order to detect and quantify the prion proteins (PrPC) onto the cell membrane using the higher binding affinity of such proteins for copper ions. A combined method of hydrothermal “green” synthesis and thermal treatment allows us to obtain impurity-free surfaces for SERS measurement, suitable for cell growth. The plasmon absorption of the gold nanostructures was monitored by UV–vis spectrometry. The most significant red shift in the longitudinal plasmon resonance absorption of gold nanostructures was maximized in order to achieve the highest electromagnetic enhancement in Raman measurements. Our SERS based optical sensor has been used to detect and quantify the PrPC –Cu2+ interaction in vitro as a function of copper concentration and time in a rat neuroblastoma cell line (B104) and in three other cell models (SH-SY5Y, GN11, HeLa), expressing PrPC at different levels. The proposed methodology can be engineered in order to obtain an extremely fast and low-cost diagnostic tool to evaluate the subject’s proneness to incur neurodegenerative processes.

Different silver nanostructures have been rapidly synthesized under microwave irradiation from a solution of silver nitrate (AgNO3) and beta-D glucose; neither additional reducing nor capping agent were required in this soft green solution approach. Not only spherical nanoparticles, but also necklace and wires have been synthesized. The plasmon resonances of the synthesized silver nanostructures were tuned by varying the irradiation time and hence by changing size and morphology of nanostructures. The obtained nanostructures were characterized by X-Ray diffraction (XRD), Uv-Vis spectroscopy (Uv-Vis), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). The change of peak position and the shape of the absorption spectra were clearly observed during the whole reaction process; in fact, it was evidenced that initially Ag nanoparticles were formed, which, as reaction time elapsed, self-assembled and fused with each other to yield nanowires.

The structural and morphological evolution of nanostructured thin films obtained from thermal evaporation of polycrystalline Sn-Se starting charge as a function of the subsequent annealing temperature in an oxygen flow has been analysed. High-resolution transmission electron microscopy, small area electron diffraction, digital image processing, x-ray diffraction and Raman spectroscopy have been employed in order to investigate the structure and the morphology of the obtained films. The results evidenced, in the temperature range from RT to 500°C, the transition of the material from a homogeneous mixture of SnSe and SnSe2 nanocrystals, towards a homogeneous mixture of SnO2 and SeO2 nanocrystals, with an intermediate stage in which only SnSe2 nanocrystals are present.

Dendritic crystalline copper selenides Cu2-xSe microstructures with various dimensions have been fabricated in large scale through thermal treatment of CuSe powder in argon flow, without any catalyst. The CuSe powder grains were used as both reagents and substrates for the growth of the Cu2-xSe dendrites. The synthesized microstructures were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, selected area diffraction pattern and Raman spectroscopy. Each individual dendrite was mainly composed of a long central trunk with secondary lateral branches. The length of the main trunk was in the range 10-30 mu m, the width of the secondary branch lay in the range 1-5 mu m. The trunk was about 1-2 mu m in diameter while the lateral branches were about 0.4-0.8 mu m in diameter. The lateral branches grew in parallel and kept about 60 degrees with respect to the central trunk. A possible growth mechanism has been also proposed to account the growth of these Cu2-xSe dendritic microstructures.

Silver nanostructures were successfully synthesized through a simple and “green” method using saccharides as reducing and capping agent. Transmission electron microscopy (TEM) and UV–Vis absorption were used to certify the quality of the silver nanoparticles obtained: first, size and dispersion. In this work Silver NanoParticles (AgNPs) cytotoxicity related to saccharides capping (Glucose and Glucose-Sucrose) was explored. Human epitheloid cervix carcinoma cells (HeLa) were used for cytotoxicity test. The cells were incubated with increasing AgNPs number/cell and HeLa cells viability was monitored for a period of 48 h compared with the positive and negative controls. We observed that the toxicity increases in a incubation time and AgNPs number/cell related manner. In addition, the AgNP-G are more toxic than AgNP-GS, suggesting that AgNPs citotoxicity could depend on the capping agent. in HeLa cells the highest AgNP-G number/cell induces , cell deathsoon after 1 hr of incubation; conversely the lowest AgNP-GS number/cell induces cell proliferation.

Exploiting the experimental factorial design and the potentiality of Turbiscan AG Station, we developed and characterized unmodified and DDAB-coated NLC prepared by a low energy organic solvent free phase inversion temperature technique. A 22 full factorial experimental design was developed in order to study the effects of two independent variables (DDAB and ferulic acid) and their interaction on mean particle size and zeta potential values. The factorial planning was validated by ANOVA analysis; the correspondence between the predicted values of size and zeta and those measured experimentally confirmed the validity of the design and the equation applied for its resolution. The DDAB-coated NLC were significantly affected in their physico-chemical properties by the presence of DDAB, as showed by the results of the experimental design. The coated NLC showed higher physical stability with no particles aggregation compared to the unmodified NLC, as demonstrated by Turbiscan (R) AGS measurements. X-ray diffraction, Raman spectroscopy and Cryo-TEM images allowed us to assert that DDAB plays a critical role in increasing the lipids structural order with a consequent enhancement of the NLC physical stability. Furthermore, the results of the in vitro biological studies allow the revisiting of the role of DDAB to the benefit of glioblastoma treatment, due to its efficacy in increasing the NLC uptake and reducing the viability of human glioblastoma cancer cells (U87MG).

During the Middle Ages in Europe, a different post-mortem funerary custom came to be used in order to transport and solemnly dispose of the bodies of high-status individuals. Because of their high degree of mobility, most medieval kings and queens rarely died where they had planned to be buried; thus, they had to be moved to the place of burial. Ancient writings describe some post-mortem funerary practices carried out to facilitate transport, such as boiling or burning of bodies after death. The remains of Henry VII of Luxembourg were analysed in order to determine which post-mortem practices were utilized. A detailed chemical-physical analysis was conducted to highlight the changes in the bone matrix due to post-mortem alteration. Boiling and burning leave different marks in the bone that could be differentiated through the analysis of the inorganic and organic components of the bone. Accordingly, anthropological, X-ray diffraction (XRD), infrared spectroscopy (FT-IR), collagen ratio, and scanning electron microscopy (FE-SEM/EDAX) analysis were performed on two different bone fragments: cranial and tibial shaft. This multidisciplinary approach has enriched scientific understanding of the post-mortem practices to which the skull and tibial shaft of Henry VII were subjected. The results highlight that the tibial shaft was treated under higher temperature respect to the skull. Furthermore, this analysis also shed light on the state of preservation of the bone fragments analysed and has allowed us to initiate more complex molecular analysis, as well as ancient DNA analysis.

A real time and sensitive methodology has been developeded and optimized to detect water soluble molecules.

Polymer supported palladium catalyst, obtained by copolymerization of Pd(AAEMA)2 [AAEMA− = deprotonated form of 2-(acetoacetoxy)ethyl methacrylate] with ethyl methacrylate (co-monomer) and ethylene glycol dimethacrylate (cross-linker), exhibited excellent activity and selectivity for the hydrogenation of quinolines to 1,2,3,4-tetrahydroquinolines under mild temperature (80 °C) and H2 pressure (10 bar) in aqueous medium. Both the activity and selectivity could be maintained for at least nine reaction runs. No metal leaching into solution occurred during application. TEM analyses carried out on the catalyst showed that the active species were supported palladium nanoparticles having a mean size of 4 nm, which did not aggregate with the recycles.