scholarly journals On the reliability of highly magnified micrographs for structural analysis in materials science

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Martin Wortmann ◽  
Ashley Stephen Layland ◽  
Natalie Frese ◽  
Uwe Kahmann ◽  
Timo Grothe ◽  
...  

Abstract Highly magnified micrographs are part of the majority of publications in materials science and related fields. They are often the basis for discussions and far-reaching conclusions on the nature of the specimen. In many cases, reviewers demand and researchers deliver only the bare minimum of micrographs to substantiate the research hypothesis at hand. In this work, we use heterogeneous poly(acrylonitrile) nanofiber nonwovens with embedded nanoparticles to demonstrate how an insufficient or biased micrograph selection may lead to erroneous conclusions. Different micrographs taken by transmission electron microscopy and helium ion microscopy with sometimes contradictory implications were analyzed and used as a basis for micromagnetic simulations. With this, we try to raise awareness for the possible consequences of cherry-picking for the reliability of scientific literature.

2015 ◽  
Vol 1132 ◽  
pp. 19-35
Author(s):  
S.O. Dozie-Nwachukwu ◽  
J.D. Obayemi ◽  
Y. Danyo ◽  
G. Etuk-Udo ◽  
N. Anuku ◽  
...  

This paper presents the biosynthesis of gold nanoparticles from the bacteria, Serratia marcescens.The intra-and extra-cellular synthesis of gold nanoparticles is shown to occur over a range of pH and incubation times in cell-free exracts and biomass ofserratia marcescensthat were reacted with 2.5mM Tetrachloroauric acid (HAuCl4). The formation of gold nanoparticles was identified initially via color changes from yellow auro-chloride to shades of red or purple in gold nanoparticle solutions. UV-Visible spectroscopy (UV-Vis), Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray spectroscopy (EDS), Helium Ion Microscopy (HIM) and Dynamic Light Scattering (DLS) were also used to characterize gold nanoparticles produced within a range of pH conditions. The results show clearly that the production of gold nanoparticles from cell-free extracts require shorter times than the production of gold nanoparticles from the biomass.


Author(s):  
Tomasz Blachowicz ◽  
Michal Koruszowic

Topothesy and fractal dimensions were calculated for poly(acrylonitrile) (PAN) nanofibers mats obtained by electrospinning. These methods enable quantitatively describing and thus comparing solid-state surfaces and detecting fabric errors. The obtained variety of structural properties results from different substrates and after-treatments, e.g. stabilization and carbonization. The change in spatial morphology was reported for different magnification of images obtained with the use of Helium Ion Microscopy (HIM).


Author(s):  
Hannes Lichte ◽  
Edgar Voelkl

The object wave o(x,y) = a(x,y)exp(iφ(x,y)) at the exit face of the specimen is described by two real functions, i.e. amplitude a(x,y) and phase φ(x,y). In stead of o(x,y), however, in conventional transmission electron microscopy one records only the real intensity I(x,y) of the image wave b(x,y) loosing the image phase. In addition, referred to the object wave, b(x,y) is heavily distorted by the aberrations of the microscope giving rise to loss of resolution. Dealing with strong objects, a unique interpretation of the micrograph in terms of amplitude and phase of the object is not possible. According to Gabor, holography helps in that it records the image wave completely by both amplitude and phase. Subsequently, by means of a numerical reconstruction procedure, b(x,y) is deconvoluted from aberrations to retrieve o(x,y). Likewise, the Fourier spectrum of the object wave is at hand. Without the restrictions sketched above, the investigation of the object can be performed by different reconstruction procedures on one hologram. The holograms were taken by means of a Philips EM420-FEG with an electron biprism at 100 kV.


Author(s):  
John F. Mansfield

One of the most important advancements of the transmission electron microscopy (TEM) in recent years has been the development of the analytical electron microscope (AEM). The microanalytical capabilities of AEMs are based on the three major techniques that have been refined in the last decade or so, namely, Convergent Beam Electron Diffraction (CBED), X-ray Energy Dispersive Spectroscopy (XEDS) and Electron Energy Loss Spectroscopy (EELS). Each of these techniques can yield information on the specimen under study that is not obtainable by any other means. However, it is when they are used in concert that they are most powerful. The application of CBED in materials science is not restricted to microanalysis. However, this is the area where it is most frequently employed. It is used specifically to the identification of the lattice-type, point and space group of phases present within a sample. The addition of chemical/elemental information from XEDS or EELS spectra to the diffraction data usually allows unique identification of a phase.


Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  

Remote on-line electron microscopy is rapidly becoming more available as improvements continue to be developed in the software and hardware of interfaces and networks. Scanning electron microscopes have been driven remotely across both wide and local area networks. Initial implementations with transmission electron microscopes have targeted unique facilities like an advanced analytical electron microscope, a biological 3-D IVEM and a HVEM capable of in situ materials science applications. As implementations of on-line transmission electron microscopy become more widespread, it is essential that suitable standards be developed and followed. Two such standards have been proposed for a high-level protocol language for on-line access, and we have proposed a rational graphical user interface. The user interface we present here is based on experience gained with a full-function materials science application providing users of the National Center for Electron Microscopy with remote on-line access to a 1.5MeV Kratos EM-1500 in situ high-voltage transmission electron microscope via existing wide area networks. We have developed and implemented, and are continuing to refine, a set of tools, protocols, and interfaces to run the Kratos EM-1500 on-line for collaborative research. Computer tools for capturing and manipulating real-time video signals are integrated into a standardized user interface that may be used for remote access to any transmission electron microscope equipped with a suitable control computer.


Author(s):  
Judith M. Brock ◽  
Max T. Otten

A knowledge of the distribution of chemical elements in a specimen is often highly useful. In materials science specimens features such as grain boundaries and precipitates generally force a certain order on mental distribution, so that a single profile away from the boundary or precipitate gives a full description of all relevant data. No such simplicity can be assumed in life science specimens, where elements can occur various combinations and in different concentrations in tissue. In the latter case a two-dimensional elemental-distribution image is required to describe the material adequately. X-ray mapping provides such of the distribution of elements.The big disadvantage of x-ray mapping hitherto has been one requirement: the transmission electron microscope must have the scanning function. In cases where the STEM functionality – to record scanning images using a variety of STEM detectors – is not used, but only x-ray mapping is intended, a significant investment must still be made in the scanning system: electronics that drive the beam, detectors for generating the scanning images, and monitors for displaying and recording the images.


2014 ◽  
pp. 32-35
Author(s):  
Teodor Paunescu ◽  
Sylvie Breton ◽  
Dennis Brown

Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1791
Author(s):  
Marco Vizcarra-Pacheco ◽  
María Ley-Flores ◽  
Ana Mizrahim Matrecitos-Burruel ◽  
Ricardo López-Esparza ◽  
Daniel Fernández-Quiroz ◽  
...  

One of the main challenges facing materials science today is the synthesis of new biodegradable and biocompatible materials capable of improving existing ones. This work focused on the synthesis of new biomaterials from the bioconjugation of oleic acid with L-cysteine using carbodiimide. The resulting reaction leads to amide bonds between the carboxylic acid of oleic acid and the primary amine of L-cysteine. The formation of the bioconjugate was corroborated by Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and nuclear magnetic resonance (NMR). In these techniques, the development of new materials with marked differences with the precursors was confirmed. Furthermore, NMR has elucidated a surfactant structure, with a hydrophilic part and a hydrophobic section. Ultraviolet-visible spectroscopy (UV-Vis) was used to determine the critical micellar concentration (CMC) of the bioconjugate. Subsequently, light diffraction (DLS) was used to analyze the size of the resulting self-assembled structures. Finally, transmission electron microscopy (TEM) was obtained, where the shape and size of the self-assembled structures were appreciated.


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