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1.
Microsc Microanal ; 2024 Mar 06.
Article in English | MEDLINE | ID: mdl-38447171

ABSTRACT

Atom probe tomography (APT) is a unique analytical technique that offers three-dimensional elemental mapping with a spatial resolution down to the sub-nanometer. When APT is applied on complex heterogenous systems and/or under certain experimental conditions, that is, laser illumination, the specimen shape can deviate from an ideal hemisphere. Insufficient consideration of this aspect can introduce artifacts in the reconstructed dataset, ultimately degrading its spatial accuracy. So far, there has been limited investigation into the detailed evolution of emitter shape and its impact on the field-of-view (FOV). In this study, we numerically and experimentally investigated the FOV for asymmetric emitters and its evolution throughout the analysis depth. Our analysis revealed that, for asymmetric emitters, the ions evaporated from the topmost region of the specimen (summit) project approximately to the detector center. Furthermore, we demonstrated the implications of this finding on the FOV location for asymmetric emitters. Based on our findings, the location of the center of the FOV can deviate from the specimen central axis with an evolution depending on the evolution of the emitter shape. This study highlights the importance of accounting for the specimen shape when developing advanced data reconstruction schemes to enhance spatial resolution and accuracy.

2.
Anal Chem ; 92(16): 11413-11419, 2020 Aug 18.
Article in English | MEDLINE | ID: mdl-32664722

ABSTRACT

With the continuous miniaturization and increasing complexity of the devices used in nanotechnology, there is a pressing need for characterization techniques with nm-scale 3D-spatial resolution. Unfortunately, techniques like Secondary Ion Mass Spectrometry (SIMS) fail to reach the required lateral resolution. For this reason, new concepts and approaches, including the combination of different complementary techniques, have been developed in over the past years to try to overcome some of the challenges. Beyond the problem of spatial resolution in a 3D SIMS experiment, one is also faced with the impact of changes in topography during the analysis. These are quite difficult to identify because they originate from the different sputter rates of the various materials and or phases in a heterogeneous system and are notorious at the interfaces between organic and inorganic layers. As each of these materials will erode at a different velocity, accurate 3D-analysis will require means to establish a spatially resolved relation between ion bombardment time and depth. Inevitably such a nonhomogeneous erosion will lead to the development of surface topography. The impact of these effects can be overcome provided one can capture the time and spatially dependent surface erosion (velocity) with high spatial resolution during the course of a profiling experiment. Incorporating a Scanning Probe Microscope (SPM) unit which provides topography measurements with high spatial resolution, into a SIMS tool (e.g., Time of Flight (ToF) SIMS) with means to alternate between SPM and SIMS measurements, is one approach to meet that demand for complementary topographical information allowing accurate 3D chemical imaging. In this paper, the result of integrating a SPM module into a ToF-SIMS system is presented illustrating the improvements in 3D data accuracy which can be obtained when analyzing complex 3D-systems.

3.
Sci Rep ; 8(1): 11305, 2018 Jul 27.
Article in English | MEDLINE | ID: mdl-30054503

ABSTRACT

Controlling the location and the distribution of hot spots is a crucial aspect in the fabrication of surface-enhanced Raman spectroscopy (SERS) substrates for bio-analytical applications. The choice of a suitable method to tailor the dimensions and the position of plasmonic nanostructures becomes fundamental to provide SERS substrates with significant signal enhancement, homogeneity and reproducibility. In the present work, we studied the influence of the long-range ordering of different flexible gold-coated Si nanowires arrays on the SERS activity. The substrates are made by nanosphere lithography and metal-assisted chemical etching. The degree of order is quantitatively evaluated through the correlation length (ξ) as a function of the nanosphere spin-coating speed. Our findings showed a linear increase of the SERS signal for increasing values of ξ, coherently with a more ordered and dense distribution of hot spots on the surface. The substrate with the largest ξ of 1100 nm showed an enhancement factor of 2.6 · 103 and remarkable homogeneity over square-millimetres area. The variability of the signal across the substrate was also investigated by means of a 2D chemical imaging approach and a standard methodology for its practical calculation is proposed for a coherent comparison among the data reported in literature.

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