Determination of the denaturation temperature of the Spike protein S1 of SARS-CoV-2 (2019 nCoV) by Raman spectroscopy.

In the present work the temperature response of the constitutive S1 segment of the SARS-CoV-2 Spike Glycoprotein (GPS) has been studied. The intensity of the Raman bands remained almost constant before reaching a temperature of 133 °C. At this temperature a significant reduction of peak intensities was observed. Above 144 °C the spectra ceased to show any recognizable feature as that of the GPS S1, indicating that it had transformed after the denaturation process that it was subjected. The GPS S1 change is irreversible. Hence, Raman Spectroscopy (RS) provides a precision method to determine the denaturation temperature (TD) of dry powder GPS S1. The ability of RS was calibrated through the reproduction of TD of other well studied proteins as well as those of the decomposition temperature of some amino acids (AA). Through this study we established a TD of 139 ± 3 °C for powder GPS S1 of SARS-CoV-2.

Order-disorder phase transitions in Au-Cu nanocubes: from nano-thermodynamics to synthesis.

Catalysts have been widely used in industries and can be optimized by tuning the composition and chemical ordering of the elements involved in the nano-alloy. Among bi-metallic alloys, the Au-Cu system is of particular interest because it exhibits ordered phases at low temperatures. Nevertheless, the temperature at which these ordered structures are formed is totally unknown at the nanoscale. Consequently, to speed up the development of these catalysts, this paper theoretically predicts the structural phase transitions between ordered and disordered phases for the Au-Cu system by using nano-thermodynamics. Following the predictions, the suggested annealing temperatures have been carefully chosen and consequently, Au-Cu ordered nanocubes have been successfully synthesized through a solventless protocol. The results are fully supported by electron microscopy observations.

Electric radiation mapping of silver/zinc oxide nanoantennas by using electron holography.

In this work, we report the fabrication of self-assembled zinc oxide nanorods grown on pentagonal faces of silver nanowires by using microwaves irradiation. The nanostructures resemble a hierarchal nanoantenna and were used to study the far and near field electrical metal-semiconductor behavior from the electrical radiation pattern resulting from the phase map reconstruction obtained using off-axis electron holography. As a comparison, we use electric numerical approximations methods for a finite number of ZnO nanorods on the Ag nanowires and show that the electric radiation intensities maps match closely the experimental results obtained with electron holography. The time evolution of the radiation pattern as generated from the nanostructure was recorded under in-situ radio frequency signal stimulation, in which the generated electrical source amplitude and frequency were varied from 0 to 5 V and from 1 to 10 MHz, respectively. The phase maps obtained from electron holography show the change in the distribution of the electric radiation pattern for individual nanoantennas. The mapping of this electrical behavior is of the utmost importance to gain a complete understanding for the metal-semiconductor (Ag/ZnO) heterojunction that will help to show the mechanism through which these receiving/transmitting structures behave at nanoscale level.

Determination of the surface morphology of gold-decahedra nanoparticles using an off-axis electron holography dual-lens imaging system.

The purpose of this paper is to show surface irregularities in gold decahedra nanoparticles extracted by using off-axis electron holography in a JEOL ARM 200F microscope. Electron holography has been used in a dual-lens system within the objective lenses: main objective lens and objective minilens. Parameters such as biprism voltage, fringe spacing (σ), fringe width (W) and optimum fringe contrast have been calibrated. The reliability of the transmission electron microscope performance with these parameters was carried out through a plug-in in the Digital-Micrograph software, which considers the mean inner potential within the particle leading a precise determination of the morphological surface of decahedral nanoparticles obtained from the reconstructed unwrapped phase and image processing. We have also shown that electron holography has the capability to extract information from nanoparticle shape that is currently impossible to obtain with any other electron microscopy technique.

Morphology control of nanostructures: Na-doped PbTe-PbS system.

The morphology of crystalline precipitates in a solid-state matrix is governed by complex but tractable energetic considerations driven largely by volume strain energy minimization and anisotropy of interfacial energies. Spherical precipitate morphologies are favored by isotropic systems, while anisotropic interfacial energies give energetic preference to certain crystallographically oriented interfaces, resulting in a faceted precipitate morphology. In conventional solid-solution precipitation, a precipitate's morphological evolution is mediated by surface anchoring of capping molecules, which dramatically alter the surface energy in an anisotropic manner, thereby providing exquisite morphology control during crystal growth. Herein, we present experimental evidence and theoretical validation for the role of a ternary element (Na) in controlling the morphology of nanoscale PbS crystals nucleating in a PbTe matrix, an important bulk thermoelectric system. The PbS nanostructures formed by phase separation from a PbI(2)-doped or undoped PbTe matrix have irregular morphologies. However, replacing the iodine dopant with Na (1-2 mol %) alters dramatically the morphology of the PbS precipitates. Segregation of Na at PbTe/PbS interfaces result in cuboidal and truncated cuboidal morphologies for PbS. Using analytical scanning/transmission electron microscopy and atom-probe tomography, we demonstrate unambiguously that Na partitions to the precipitates and segregates at the matrix/precipitate interfaces, inducing morphological anisotropy of PbS precipitates. First-principles and semiclassical calculations reveal that Na as a solute in PbTe has a higher energy than in PbS and that Na segregation at a (100) PbTe/PbS interface decreases the total energy of matrix/precipitate system, resulting in faceting of PbS precipitates. These results provide an impetus for a new strategy for controlling morphological evolution in matrix/precipitate systems, mediated by solute partitioning of ternary additions.

Microwave-assisted synthesis of gold nanoparticles self-assembled into self-supported superstructures.

Passivated gold nanoparticles were synthesized through a microwave-assisted process in a two-phase system, in the presence of 1-dodecanethiol. An average particle size of 1.8 nm of the gold nanoparticles obtained and 0.35 S.D. was determined through HRTEM and STEM analysis. It was observed that these nanoparticles spontaneously self-assemble into self-supported superstructures of 1 µm in diameter avg and 400 nm thickness, yielding an off-white powder which can be handled as a simple powder. XRD analysis indicates that n-alkanethiol molecules used as a passivating compound, besides protecting against crystal growth, interact to form cubic ordered arrays between the nanoparticles. This interaction leads to the superstructure formation, with an average distance between nanoparticles in the array, of 3.56 nm. Theoretical calculations and molecular dynamics simulations were performed to analyze the resulting structure.

Structural characterization of Pt-Pd core-shell nanoparticles by Cs-corrected STEM.

Pt-Pd core-shell nanoparticles were synthesized using a modified polyol method. A thermal method under refluxing, carrying on the reaction up to 285 °C, has been performed to reduce metallic salts using ethylene glycol as reducer and poly(N-vinyl-2-pyrrolidone) as protective reagent of the formed bimetallic nanoparticles. According to other works, this type of structure has been studied and utilized to successfully increase the catalytic properties of monometallic nanoparticles Pt or Pd. Core-shell bimetallic nanoparticles were structurally characterized using aberration-corrected scanning transmission electron microscopy (Cs-STEM) equipped with a high-angle annular dark field detector, energy-dispersive X-ray spectrometry (EDS), and electron energy-loss spectroscopy (EELS). The high-resolution elemental line scan and mappings were carried out using a combination of STEM-EDS and STEM-EELS. The obtained results show the growth of the Pd shell on the Pt core with polyhedral morphology. The average size of the bimetallic nanoparticles was 13.5 nm and the average size of the core was 8.5 nm; consequently, the thickness of the shell was around 2.5 nm. The growth of the Pd shell on the Pt core is layer by layer, suggesting a Frank-van der Merwe growth mechanism.

Synthesis and structural characterization of Mo-Ni-W oxide nanostructures.

In this work, we report the synthesis and characterization of Mo-Ni-W oxides. The precursor was prepared from an aqueous solution of ammonium heptamolibdate, ammonium metatungstate, and nickel nitrate with an atomic ratio of 1:1:1 (Mo:W:Ni). The solution was then transferred to a Teflon-lined stainless steel autoclave and heated to 200 degrees C and left at this temperature for 48 h. The resulting material was then washed and dried. The morphology and elemental composition were studied by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. The porosity was studied by the Brunauer, Emmett, and Teller method. The materials synthesized at 200 degrees C remained amorphous and had a specific surface area of 114 m2/g with pore size of 34 A. The average length was 1 microm and the average diameter was 60 nm. The crystalline phase of synthesized material corresponded to W0.4Mo0.6O3 and WO3. After annealing at 550 degrees C for two hours, the material was polycrystalline with a segregated structure of MoO3, WO3; NiMoO4 was observed. The sublimation of the molybdenum oxide was evident when annealed at 900 degrees C for two hours and finally two crystalline phases of material remained; roundish WO3 and elongated particles of NiWO4.

On the interpretation of the forbidden spots observed in the electron diffraction patterns of flat Au triangular nanoparticles.

In many cases nanostructures present forbidden spots in their electron diffraction patterns when they are observed by transmission electron microscopy (TEM). To interpret their TEM and high resolution transmission electron microscopy (HRTEM) images properly, an understanding of the origin of these spots is necessary. In this work we comment on the origin of the forbidden spots observed in the [111] and [112] electron diffraction patterns of flat gold triangular nanoparticles. The forbidden spots were successfully indexed as corresponding to the first laue Zone (FOLZ) and the HRTEM images presented a contrast produced by the interference of the zero-order Laue zone (ZOLZ) and FOLZ spots. We discuss the use of the forbidden spots in the study of the structure of nanoparticles and show that they are related to the shape and incompleteness of layers in the very thin particles.

Highly size-controlled synthesis of Au/Pd nanoparticles by inert-gas condensation.

Gold/Palladium nanoparticles were fabricated by inert-gas condensation on a sputtering reactor. With this method, by controlling both the atmosphere on the condensation chamber and the magnetron power, it was possible to produce nanoparticles with a high degree of monodispersity in size. The structure and size of the Au/Pd nanoparticles were determined by mass spectroscopy, and confirmed by atomic force microscopy and electron transmission microscopy measurements. The chemical composition was analyzed by X-ray microanalysis. From these measurements we confirmed that with the sputtering technique we are able to produce particles of 1, 3, and 5 nm on size, depending on the choice of the synthesis conditions. From TEM measurements made both in the regular HREM, as well as in STEM-HAADF mode, we found that the particles are icosahedral in shape, and the micrographs show no evidence of a core-shell structure, in contrast to what is observed in the case of nanoparticles prepared by chemical synthesis.

Ti, Ni and TiNi nanoparticles physically synthesized by Ar+ beam milling.

When the size of a particle decreases around 100 nm or less, there is a change in properties from those shown in the bulk material. In this work approximately 3 nm nanoparticles of Ni, Ti and TiNi bimetallic are produced using physical vapor deposition (PVD). Nanoparticles are characterized by High Resolution Transmission Electron Microscopy (HRTEM), High Angle Annular Dark Field (HAADF), Electron Diffraction (ED). The results show that all nanoparticles maintain the same crystal structure of bulk material but a change in their lattice parameter is produced.

Three-layer core/shell structure in Au-Pd bimetallic nanoparticles.

This paper describes the internal structure of Au-Pd nanoparticles exhibiting newly discovered three-layer core/shell morphology, which is composed of an evenly alloyed inner core, an Au-rich intermediate layer, and a Pd-rich outer shell. By exploitation of spatially resolved imaging and spectroscopic and diffraction modes of transmission electron microscopy (TEM), insights were gained on the composition of each one of the observed three layers, indicating a significant extent of intimate alloy among the monometallic elements.

Evidence of the interaction of evaporated Pt nanoparticles with variously treated surfaces of highly oriented pyrolytic graphite.

The interactions of Pt nanoparticles, deposited by evaporation onto highly oriented pyrolytic graphite surfaces modified by kiloelectronvolt Ar+ beam treatment, have been studied by X-ray photoelectron spectroscopy core-level line shape analysis. The C1s and Pt4f7/2 peaks were each considered to be composed of one asymmetric peak, and changes in their asymmetry parameters were used to study their interfacial interactions. In addition to these changes, strong signal intensity changes with time were found for both the C1s and Pt4f peaks, indicating an initial crystalline orientational instability of the Pt nanoparticles, which is supported by time-dependent high-resolution electron microscopy studies at elevated temperatures.

Surface diffusion and coalescence of mobile metal nanoparticles.

The diffusion and coalescence of metal nanoparticles play important roles in many phenomena. Here, we offer a new integrated overview of the main factors that control the nanoparticle coalescence process. Three factors are considered in our description of the coalescence process: nanoparticle diffusion across the surface, their physical and thermodynamic properties, and the mechanism of coalescence. We demonstrate that the liquid-like properties of the surface layers of the nanoparticles play an essential role in this process. We present experimental evidence for our opinion, based on the high-resolution electron microscopic analysis of several different types of nanoparticles.

Surface reconstruction and decahedral structure of bimetallic nanoparticles.

We report on energetic surface reconstruction phenomena observed on bimetallic nanoparticle systems of AuPd and AuCu, similar to a resolidification effect observed during the cooling process in lead clusters. These binary alloy nanoparticles show the fivefold edges truncated, resulting in [100] facets on decahedral structures, an effect largely envisioned and reported theoretically, with no experimental evidence so far. We demonstrate experimentally as well as by computational simulations that this new eutectic structure is favored in such nanoalloy systems.

Observation of sulfur on the surface of giant aurothiol nanoclusters.

We report the study of aurothiol nanoclusters using high-resolution electron microscopy, energy loss spectroscopy, X-ray photoelectron spectroscopy, Auger spectroscopy, and microscopy. It is concluded that the sulfur atoms are located on the surface of the gold nanoparticles in both (100) and (111) microfacets. The X-ray photoelectron spectroscopy data show that there is a Au-Au bond as well as a Au-S bond. Auger depth profile measurements made by sputtering of the nanoparticles corroborates that the sulfur is located on the surface of the nanoparticle. Quantitative Auger analysis indicates a ratio Au/S between approximately 1.79 and 1.98.

Synthesis and characterization of quantum dot superlattices.

Gold nanoparticles have been synthesized using n-alkylthiol molecules as a passivating agent. By fixing the length of the thiol chain, it is possible to produce nanocrystal arrays, such as 1D chains, 2D arrays of chains and 3D crystals.

[Otosclerosis and Van der Hoeven's syndrome: a contribution]. / Aportación al estudio de la otosclerosis y del síndrome de Van der Hoeve.

Morphological and microchemical changes that effect to the otosclerotic stape in the Van der Hoeve's syndrome were examined with a scanning electron microscope equipped with an energy dispersive X-ray fluorescence. Using the Ca/P ratio as criterion--measured by the characteristic x-ray fluorescence--it was shown that the Van der Hoeve stape had a higher Ca/P ratio (2.6:1) as compared to the normal stape (2:1). The Van der Hoeve's syndrome lesions as poorly mineralized, with low calcium salt and apparent increase of phosphates. This finding indicates a possible change from hydroxyapatite (or apatite) to brushite, which imply an acidification of bone.

Aportación al estudio de la otosclerosis y del síndrome de Van der Hoeve / Otosclerosis and Van der Hoeve's syndrome: a contribution

Hemos realizado un estudio ultraestructural y microanalítico de estribos procedentes de pacientes otosclerosos, sanos y afectos por el síndrome de Van der Hoeve a fin de determinar los cambios en la composición mineral de los mismos. Para ello hemos utilizado métodos no destructivos microscopía electrónica de barrido asociado a espectroscopia por dispersión de energía de rayos X (EDAX)- y otros destructivos (espectrografía con infrarrojos mediante transformada de Fourier). Utilizando la relación Ca/P hemos determinado que la composición mineral de los estribos es distinta en individuos normales, otosclerosos y afectos por el síndrome de Van der Hoeve. En esta última entidad hemos detectado una composición mineral inusual en huesos sanos: la brushita (AU)

Morphological and microchemical changes that effect to the otosclerotic stape in the Van der Hoeve's syndrome were examined with a scanning electron microscope equipped with an energy dispersive X-ray fluorescence. Using the Ca/P ratio as criterion--measured by the characteristic x-ray fluorescence--it was shown that the Van der Hoeve stape had a higher Ca/P ratio (2.6:1) as compared to the normal stape (2:1). The Van der Hoeve's syndrome lesions as poorly mineralized, with low calcium salt and apparent increase of phosphates. This finding indicates a possible change from hydroxyapatite (or apatite) to brushite, which imply an acidification of bone (AU)

Scanning electron microscopy images and energy-dispersive X-ray microanalysis of the stapes in otosclerosis and Van der Hoeve syndrome.

OBJECTIVE/HYPOTHESIS: The objective of this study was to evaluate the morphological and microchemical changes that affect sclerotic stapes in otospongiosis and van der Hoeve syndrome. METHODS: A scanning electron microscope equipped with an energy-dispersive x-ray analyzer was used in the experiments. RESULTS: In otosclerosis, focal lesions are poorly mineralized, with low calcium salt and reduced calcium-to-phosphorus (Ca/P) ratio (1.9:1). This finding correlates with a spongiotic type of lesion and indicates unstable mineralization with possible change from hydroxyapatite to calcium triphosphate. In van der Hoeve syndrome the presence of magnesium in stapes suggests osteoclastic function stimulation. The osteoclasts secrete many protons, causing an acidified microenvironment. Brushite is formed, and Ca/P ratio decreases in comparison with that of control patients (2.0:1 vs. 2.6:1).