Identification of nano-phases: relative merit of local analysis techniques (HRTEM, nanodiffraction, EDS/EELS) (original) (raw)

Quantitative nanoscale characterisation by electron microscopy

ABSTRACT: The transmission electron microscope (TEM) is a choice instrument for the characterisation of materials and devices at the nanoscale. Apart from high spatial resolution, TEM offers a number of signals which can be exploited to obtain chemical and structural information concerning the specimen. Recent years have seen considerable advances in the use of electron microscopy and new techniques have been developed thanks to improved methodology, instrumentation and data acquisition systems.

Nano Phase Characterization by Transmission Electron Microscopy: Experimental and Simulation

Materials Sciences and Applications, 2015

This paper introduces a methodology of characterization of nanostructured systems in which transmission electron microscopy is used as a central element of the study. Experimental studies of HREM are performed in parallel with studies in the Simula TEM program to stimulate high-resolution images and diffraction patterns. To confirm the accuracy of the results, studies of X-ray diffraction (XRD) were performed. In order to illustrate the methodology, bismuth oxide Bi2O3 nanoparticles are synthesized by a method of biosynthesis because this sample is rich in structural information.

Transmission Electron Microscopy of Nanomaterials

Electron Crystallography

Structural and analytical characterization, in the nanometer scale, has become very important for all types of materials in recent years. Transmission electron microscope (TEM) is a perfect instrument for this purpose, which is summarized in this chapter. Parameters such as particle size, grain size, lattice type, morphological information, crystallographic details, chemical composition, phase-type, and distribution can be obtained by transmission electron micrographs. Electron diffraction patterns of nanomaterials are also used to acquire quantitative information containing size, phase identification, orientation relationship and crystal defects in the lattice structure, etc. In this chapter, typical electron diffraction, highresolution transmission and scanning transmission electron microscope imaging in materials research, especially in the study of nanoscience are presented.

Ab initio determination of solid-state nanostructure

Nature, 2006

Advances in materials science and molecular biology followed rapidly from the ability to characterize atomic structure using single crystals 1-4 . Structure determination is more difficult if single crystals are not available 5 . Many complex inorganic materials that are of interest in nanotechnology have no periodic long-range order and so their structures cannot be solved using crystallographic methods 6 . Here we demonstrate that ab initio structure solution of these nanostructured materials is feasible using diffraction data in combination with distance geometry methods. Precise, sub-ångström resolution distance data are experimentally available from the atomic pair distribution function (PDF) 6,7 . Current PDF analysis consists of structure refinement from reasonable initial structure guesses 6,7 and it is not clear, a priori, that sufficient information exists in the PDF to obtain a unique structural solution. Here we present and validate two algorithms for structure reconstruction from precise unassigned interatomic distances for a range of clusters. We then apply the algorithms to find a unique, ab initio, structural solution for C 60 from PDF data alone. This opens the door to subångström resolution structure solution of nanomaterials, even when crystallographic methods fail.

Structural fingerprinting in the transmission electron microscope: Overview and opportunities to implement enhanced strategies for nanocrystal identification

Zeitschrift Fur Kristallographie, 2007

This paper illustrates the prospective need for structural fingerprinting methods for nanocrystals. A review of the existing fingerprinting methods for crystal structures by means of transmission electron microscopy which work for a single setting of the specimen goniometer is given. Suggestions are made on how some of these methods could be enhanced when nanocrystals and novel instrumentation are involved, i.e. when either the kinematic or quasi-kinematic scattering approximations are sufficiently well satisfied. A novel strategy for lattice-fringe fingerprinting of nanocrystals from Fourier transforms of high-resolution phase contrast transmission electron microscopy images is briefly outlined. Nanocrystal structure specific limitations to the application of this strategy are discussed. An appeal is made to share the structural data of nanocrystals freely over the internet and infrastructure that would allow this sharing is mentioned. A shorter version of this paper has been accepted for publication in a special issue on the Structure of Nanocrystals of the Zeitschrift fuer Kristallographie, International journal for structural, physical, and chemical aspects of crystalline materials.

Automated nanocrystal orientation and phase mapping in the transmission electron microscope on the basis of precession electron diffraction

Zeitschrift Fur Kristallographie, 2010

An automated technique for the mapping of nanocrystal phases and orientations in a transmission electron microscope is described. It is primarily based on the projected reciprocal lattice geometry that is extracted from electron diffraction spot patterns. Precession electron diffraction patterns are especially useful for this purpose. The required hardware allows for a scanning-precession movement of the primary electron beam on the crystalline sample and can be interfaced to any older or newer mid-voltage transmission electron microscope (TEM). Experimentally obtained crystal phase and orientation maps are shown for a variety of samples. Comprehensive commercial and open-access crystallographic databases may be used in support of the nanocrystal phase identification process and are briefly mentioned.