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1.
Materials (Basel) ; 16(22)2023 Nov 08.
Artículo en Inglés | MEDLINE | ID: mdl-38005006

RESUMEN

Testing shear-resisting plates in steel connections is one of the most challenging laboratory undertakings in steel construction, as the most common experimental layout design includes simulating the connection with its adjoining members. This significant hindrance gained particular magnitude as the need to test prototypes of topologically optimised shear cover plates became more pressing. Indeed, new code-compliant topology optimisation approaches for steel construction have recently been offered, and physically non-linear analyses have been demonstrated to be vital for assessing these elements. Hence, a rapid and reliable experimental process has become a fundamental necessity. To answer this need, a novel layout is herein proposed, in which topologically optimised and previously numerically examined bolted shear plates of a well-known steel joint were tested. The results allowed for the definition of the material trilinear model for use in subsequent numerical analysis, as well as the validation of the numerical simulation results. The discrepancy between the previously mathematically anticipated and empirically determined ultimate resistance did not exceed 1.7%.

5.
Ultramicroscopy ; 234: 113477, 2022 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-35123207

RESUMEN

High-resolution STEM-EELS provides information about the composition of crystalline materials at the atomic scale, though a reliable quantitative chemical analysis is often hampered by zone axis conditions, where neighbouring atomic column intensities contribute to the signal at the probe position. In this work, we present a procedure to determine the concentration of two elements within equivalent atomic columns from EELS elemental maps - in our case barium and lanthanum within the A-sites of Ba1.1La1.9Fe2O7, a second order Ruddlesden-Popper phase. We took advantage of the large changes in the elemental distribution from column to column and introduced a technique, which substitutes inelastic scattering cross sections during the quantification step by using parameters obtained from the actual experiment. We considered channelling / de-channelling effects via inelastic multislice simulations and were thereby able to count occupancies in each atomic column. The EELS quantification results were then used as prior information during the Rietveld refinement in XRD measurements in order to differentiate between barium and lanthanum.

6.
Ultramicroscopy ; 212: 112942, 2020 May.
Artículo en Inglés | MEDLINE | ID: mdl-32114314

RESUMEN

Direct electron detectors (DeDs) have been widely used for imaging studies because of their higher beam sensitivity, lower noise, improved pixel resolution, etc. However, there have been limited studies related to the performance in spectroscopic applications for the direct electron detection. Hereby, taking the advantage of the DeD installed on a high-performance electron energy-loss spectrometer, we systematically studied the performance of a DeD (Gatan's K2 IS) fitted on an aberration-corrected transmission electron microscope (TEM) equipped with an electron monochromator. Using SrTiO3 as the model system, the point spread function in the zero-loss region of the spectrum and the performance for core loss spectroscopy have been investigated under both 200 kV and 80 kV operating conditions. We demonstrate that the K2 detector can achieve an overall better performance at 200 kV than a charge coupled device (CCD) detector. At 80 kV, the K2 DeD is still better than a CCD, except for the relative broad tails of the zero-loss peak. The signal-to-noise ratio is very close for DeD and CCD under 80 kV. Based on our data obtained at different operating voltages, it is clear that DeD will benefit the microscopy community and boost the development of cutting-edge materials science studies by pushing the frontiers in electron energy-loss spectroscopy.

7.
Sci Rep ; 9(1): 19264, 2019 Dec 17.
Artículo en Inglés | MEDLINE | ID: mdl-31848357

RESUMEN

We have investigated the structure and chemical composition of nanoparticles synthesized by thermal decomposition of a mixture of iron oleate and manganese oleate in a high-boiling solvent in the presence of Na-oleate and oleic acid as surfactants by analytical transmission electron microscopy (TEM). The particles appear core-shell like in bright field TEM images. Higher spatial resolution TEM (HRTEM) analysis reveals a FeO/MnO like structure in the core and a spinel like structure in the shell. With high-resolution analytical methods like energy dispersive x-ray spectroscopy (EDS) and electron energy loss spectroscopy (EELS), the distribution of the metals Mn and Fe was investigated. Differences in the oxidation state of these metals were found between the core and the shell region. The presence of sodium from the used surfactant (Na-oleate) on the surface of the particles has been proved.

8.
Nanoscale ; 11(31): 14698-14706, 2019 Aug 08.
Artículo en Inglés | MEDLINE | ID: mdl-31343043

RESUMEN

Two-dimensional (2D) materials provide a plethora of novel condensed matter physics and are the new playground in materials science, offering potentially vast applications. One of the critical hurdles for many 2D systems is the synthesis of these low-dimensional systems as well as the prediction and identification of new candidates. Herein, a self-assembly of a monolayer tellurene by bonding CdTe wafers is demonstrated for the first time. The conventional applications of wafer-bonding range from the production of microelectromechanical systems to the synthesis of lattice-mismatched multi-junction photovoltaics. Due to the heterogeneous materials that are typically employed, the bond-interface usually contains a thin amorphous layer or arrays of dislocations. Such an interface is thus itself inactive and in many cases has detrimental effects on the device. The new material phase stabilized in this work consists of an undulating monolayer of tellurium atoms covalently bonded to {111} Cd-terminated CdTe wafer surfaces. First-principles calculations and experimentally observed changes in the localized plasmon excitation energy indicate the clear rearrangement of the underlying band-structure suggesting a metallic character, bands showing linear dispersion, and a significant asymmetric spin-band splitting. The I-V characteristics show the presence of a highly conductive pathway that lowers the resistivity by three orders of magnitude, as compared to bulk CdTe, which can be attributed to the tellurium monolayer. The findings indicate that suitably chosen crystallographic wafer surfaces can act as structural templates allowing the production of exotic phases. The presently stabilized monolayer is an addition to the family of tellurene variants, providing new insights into the fundamental properties of this and other emerging 2D materials, while attracting attention to the unusual side of the wafer-bonding technology exemplified in this study.

9.
Microsc Microanal ; 25(1): 80-91, 2019 02.
Artículo en Inglés | MEDLINE | ID: mdl-30698125

RESUMEN

Adding Au to Pd nanoparticles (NPs) can impart high catalytic activity with respect to hydrogenation of a wide range of substances. These materials are often synthesized by reducing metallic precursors; hence, sonochemical and solvothermal processes are commonly used to anchor these bimetals onto thin supports, including graphene. Although similar NPs have been studied reasonably well, a clear understanding of structural characteristics relative to their synthesis parameters is lacking, due to limitations in characterization techniques, which may prevent optimization of this very promising catalyst. In this report, a strategic approach has been used to identify this structural and material synthesis correlation, starting with controlled sample preparation and followed by detailed characterization. This includes advanced scanning transmission electron microscopy and electron energy loss spectroscopy; the latter using a state-of-the-art instrumentation to map the distribution of Pd and Au, and to identify chemical state of the Pd NPs, which has not been previously reported. Results show that catalytic bimetal NP clusters were made of small zero-valent Pd NPs aggregating to form a shell around an Au core. Not only can the described characterization approach be applied to similar material systems, but the results can guide the optimization of the synthesis procedures.


Asunto(s)
Catálisis , Oro/química , Grafito/química , Nanopartículas del Metal/química , Paladio/clasificación , Estructura Molecular , Tamaño de la Partícula , Solventes , Propiedades de Superficie
10.
Sci Rep ; 7(1): 8243, 2017 08 15.
Artículo en Inglés | MEDLINE | ID: mdl-28811485

RESUMEN

In many cases, electron counting with direct detection sensors offers improved resolution, lower noise, and higher pixel density compared to conventional, indirect detection sensors for electron microscopy applications. Direct detection technology has previously been utilized, with great success, for imaging and diffraction, but potential advantages for spectroscopy remain unexplored. Here we compare the performance of a direct detection sensor operated in counting mode and an indirect detection sensor (scintillator/fiber-optic/CCD) for electron energy-loss spectroscopy. Clear improvements in measured detective quantum efficiency and combined energy resolution/energy field-of-view are offered by counting mode direct detection, showing promise for efficient spectrum imaging, low-dose mapping of beam-sensitive specimens, trace element analysis, and time-resolved spectroscopy. Despite the limited counting rate imposed by the readout electronics, we show that both core-loss and low-loss spectral acquisition are practical. These developments will benefit biologists, chemists, physicists, and materials scientists alike.

11.
Micron ; 96: 29-37, 2017 May.
Artículo en Inglés | MEDLINE | ID: mdl-28226270

RESUMEN

STEM spectrum-imaging with collecting EDX signal is considered in view of the extraction of maximum information from very noisy data. It is emphasized that spectrum-images with weak EDX signal often suffer from information loss in the course of PCA treatment. The loss occurs when the level of random noise exceeds a certain threshold. Weighted PCA, though potentially helpful in isolation of meaningful variations from noise, might provoke the complete loss of information in the situation of weak EDX signal. Filtering datasets prior PCA can improve the situation and recover the lost information. In particular, Gaussian kernel filters are found to be efficient. A new filter useful in the case of sparse atomic-resolution EDX spectrum-images is suggested.

12.
Adv Mater ; 29(7)2017 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-27918114

RESUMEN

Arsenic-free drinking water, independent of electrical power and piped water supply, is possible only through advanced and affordable materials with large uptake capacities. Confined metastable 2-line ferrihydrite, stable at ambient temperature, shows continuous arsenic uptake in the presence of other complex species in natural drinking water and an affordable water-purification device is made using the same.

13.
14.
Micron ; 86: 22-9, 2016 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-27124585

RESUMEN

The elemental distribution of a precipitate cross section, situated in a lean Al-Mg-Si-Cu-Ag-Ge alloy, has been investigated in detail by electron energy loss spectroscopy (EELS) and aberration corrected high angle annular dark field scanning transmission electron microscopy (HAADF-STEM). A correlative analysis of the EELS data is connected to the results and discussed in detail. The energy loss maps for all relevant elements were recorded simultaneously. The good spatial resolution allows elemental distribution to be evaluated, such as by correlation functions, in addition to being compared with the HAADF image. The fcc-Al lattice and the hexagonal Si-network within the precipitates were resolved by EELS. The combination of EELS and HAADF-STEM demonstrated that some atomic columns consist of mixed elements, a result that would be very uncertain based on one of the techniques alone. EELS elemental mapping combined with a correlative analysis have great potential for identification and quantification of small amounts of elements at the atomic scale.

15.
Sci Rep ; 6: 23628, 2016 Mar 24.
Artículo en Inglés | MEDLINE | ID: mdl-27009604

RESUMEN

Cooperative phenomena arising due to the coupling of individual atoms via the radiation field are a cornerstone of modern quantum and optical physics. Recent experiments on x-ray quantum optics added a new twist to this line of research by exploiting superradiance in order to construct artificial quantum systems. However, so far, systematic approaches to deliberately design superradiance properties are lacking, impeding the desired implementation of more advanced quantum optical schemes. Here, we develop an analytical framework for the engineering of single-photon superradiance in extended media applicable across the entire electromagnetic spectrum, and show how it can be used to tailor the properties of an artificial quantum system. This "reverse engineering" of superradiance not only provides an avenue towards non-linear and quantum mechanical phenomena at x-ray energies, but also leads to a unified view on and a better understanding of superradiance across different physical systems.

16.
ACS Nano ; 10(2): 2406-14, 2016 Feb 23.
Artículo en Inglés | MEDLINE | ID: mdl-26816347

RESUMEN

Among the different synthesis approaches to colloidal nanocrystals, a recently developed toolkit is represented by cation exchange reactions, where the use of template nanocrystals gives access to materials that would be hardly attainable via direct synthesis. Besides, postsynthetic treatments, such as thermally activated solid-state reactions, represent a further flourishing route to promote finely controlled cation exchange. Here, we report that, upon in situ heating in a transmission electron microscope, Cu2Se or Cu nanocrystals deposited on an amorphous solid substrate undergo partial loss of Cu atoms, which are then engaged in local cation exchange reactions with Cu "acceptor" phases represented by rod- and wire-shaped CdSe nanocrystals. This thermal treatment slowly transforms the initial CdSe nanocrystals into Cu(2-x)Se nanocrystals, through the complete sublimation of Cd and the partial sublimation of Se atoms. Both Cu "donor" and "acceptor" particles were not always in direct contact with each other; hence, the gradual transfer of Cu species from Cu2Se or metallic Cu to CdSe nanocrystals was mediated by the substrate and depended on the distance between the donor and acceptor nanostructures. Differently from what happens in the comparably faster cation exchange reactions performed in liquid solution, this study shows that slow cation exchange reactions can be performed at the solid state and helps to shed light on the intermediate steps involved in such reactions.

17.
Phys Rev Lett ; 112(19): 193601, 2014 May 16.
Artículo en Inglés | MEDLINE | ID: mdl-24877939

RESUMEN

The collective emission from a one-dimensional chain of interacting two-level atoms is investigated. We calculate the light scattered by dissipative few-excitation eigenstates in the far field, and, in particular, focus on signatures of a lattice two-body bound state. We present analytical results for the angle-resolved, temporal decay of the scattered light intensity. Moreover, we find that the steady-state emission spectrum that emerges when the system is probed by a weak, incoherent driving field exhibits a distinct signature for the existence of a bound state, and allows us to determine the momentum distribution of the two-body relative wave function. Intriguingly, our study does not rely on single-atom addressability and/or manipulation techniques.

18.
Microsc Microanal ; 20(3): 779-83, 2014 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-24666478

RESUMEN

We report the analysis of the changes in local carbon structure and chemistry caused by the self-implantation of carbon into diamond via electron energy-loss spectroscopy (EELS) plasmon energy shifts and core-edge fine structure fingerprinting. These two very different EELS energy and intensity ranges of the spectrum can be acquired under identical experimental conditions and nearly simultaneously using specially designed deflectors and energy offset devices known as "DualEELS." In this way, it is possible to take full advantage of the unique and complementary information that is present in the low- and core-loss regions of the EELS spectrum. We find that self-implanted carbon under the implantation conditions used for the material investigated in this paper creates an amorphous region with significant sp 2 content that varies across the interface.

19.
Microsc Microanal ; 19(2): 487-95, 2013 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-23458469

RESUMEN

We report the installation and performance evaluation of a probe aberration-corrected high-resolution JEOL JEM-ARM200F transmission electron microscope (TEM). We provide details on construction of the room that enables us to obtain scanning transmission electron microscope (STEM) data without any evident distortions/noise from the external environment. The microscope routinely delivers expected performance. We show that the highest STEM spatial resolution and energy resolution achieved with this microscope are 0.078 nm and 0.34 eV, respectively. We report a direct comparative evaluation of the performance of this microscope with a Schottky thermal field-emission gun versus a cold field-emission gun. Cold field-emission illumination improves spatial resolution of the high current probe for analytical spectroscopy, the TEM information limit, and the electron energy resolution compared to the Schottky thermal field-emission source.

20.
Opt Express ; 20(11): 12326-40, 2012 May 21.
Artículo en Inglés | MEDLINE | ID: mdl-22714220

RESUMEN

The Hong-Ou-Mandel effect is studied in the context of two-photon transport in a one-dimensional waveguide with a single scatterer. We numerically investigate the scattering problem within a time-dependent, wave-function-based framework. Depending on the realization of the scatterer and its properties, we calculate the joint probability of finding both photons on either side of the waveguide after scattering. We specifically point out how Hong-Ou-Mandel interferometry techniques could be exploited to identify effective photon-photon interactions which are mediated by the scatterer. The Hong-Ou-Mandel dip is discussed in detail for the case of a single two-level atom embedded in the waveguide, and dissipation and dephasing are taken into account by means of a quantum jump approach.


Asunto(s)
Modelos Teóricos , Fotones , Refractometría/métodos , Simulación por Computador , Luz , Dispersión de Radiación
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