An Environmental Transmission Electron Microscope for in situ Synthesis and Characterization of Nanomaterials

2005 ◽  
Vol 20 (7) ◽  
pp. 1695-1707 ◽  
Author(s):  
Renu Sharma

The world of nanomaterials has become the real world for most applications in the area of nanotechnology. As postsynthesis handling of materials at the nanoscale level is impractical, nanomaterials must be synthesized directly as part of a device or circuit. The demands of nanotechnology have led to modifications in the design of transmission electron microscopes (TEMs) that enable in situ synthesis and characterization simultaneously. The environmental TEM (ETEM) is one such modified instrument that has often been used to follow gas–solid and/or liquid–solid interactions at elevated temperatures. Although the history and development of the ETEM, also called the controlled atmosphere or environmental cell TEM, is as old as transmission electron microscopy itself, developments in the design of medium-voltage TEMs have succeeded in bringing resolutions down to the subnanometer level. A modern ETEM equipped with a field-emission gun, energy filter or electron energy-loss spectrometer, scanning transmission electron microscopy coils, and bright-field and dark-field detectors can be a versatile tool for understanding chemical processes at the nanometer level. This article reviews the design and operations of a dedicated ETEM. Its applications range from the in situ characterization of reaction steps, such as oxidation-reduction and hydroxylation, to the in situ synthesis of nanomaterials, such as quantum dots and carbon nanotubes. Some examples of the current and the future applications for the synthesis and characterization of nanomaterials are also discussed.

2020 ◽  
Vol 75 (11) ◽  
pp. 913-919
Author(s):  
Frank Krumeich

AbstractSince the 1970s, high-resolution transmission electron microscopy (HRTEM) is well established as the most appropriate method to explore the structural complexity of niobium tungsten oxides. Today, scanning transmission electron microscopy (STEM) represents an important alternative for performing the structural characterization of such oxides. STEM images recorded with a high-angle annular dark field (HAADF) detector provide not only information about the cation positions but also about the distribution of niobium and tungsten as the intensity is directly correlated to the local scattering potential. The applicability of this method is demonstrated here for the characterization of the real structure of Nb7W10O47.5. This sample contains well-ordered domains of Nb8W9O47 and Nb4W7O31 besides little ordered areas according to HRTEM results. Structural models for Nb4W7O31 and twinning occurring in this phase have been derived from the interpretation of HAADF-STEM images. A remarkable grain boundary between well-ordered domains of Nb4W7O31 and Nb8W9O47 has been found that contains one-dimensionally periodic features. Furthermore, short-range order observed in less ordered areas could be attributed to an intimate intergrowth of small sections of different tetragonal tungsten bronze (TTB) based structures.


2012 ◽  
Vol 174-177 ◽  
pp. 508-511
Author(s):  
Lin Lin Yang ◽  
Yong Gang Wang ◽  
Yu Jiang Wang ◽  
Xiao Feng Wang

BiFeO3 polyhedrons had been successfully synthesized via a hydrothermal method. The as-prepared products were characterized by power X-ray diffraction (XRD) pattern, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The possible mechanisms for the formation of BiFeO3 polyhedrons were discussed. Though comparison experiments, it was found that the kind of precursor played a key role on the morphology control of BiFeO3 crystals.


2011 ◽  
Vol 415-417 ◽  
pp. 617-620 ◽  
Author(s):  
Yan Su ◽  
Ying Yun Lin ◽  
Yu Li Fu ◽  
Fan Qian ◽  
Xiu Pei Yang ◽  
...  

Water-soluble gold nanoparticles (AuNPs) were prepared using 2-mercapto-4-methyl-5- thiazoleacetic acid (MMTA) as a stabilizing agent and sodium borohydride (NaBH4) as a reducing agent. The AuNPs product was analyzed by transmission electron microscopy (TEM), UV-vis absorption spectroscopy and Fourier transform infrared spectroscopy (FTIR). The TEM image shows that the particles were well-dispersed and their average particle size is about 5 nm. The UV-vis absorption and FTIR spectra confirm that the MMTA-AuNPs was stabilized by the carboxylate ions present on the surface of the AuNPs.


2015 ◽  
Vol 21 (6) ◽  
pp. 1622-1628 ◽  
Author(s):  
Jonathan P. Winterstein ◽  
Pin Ann Lin ◽  
Renu Sharma

AbstractIn situenvironmental transmission electron microscopy (ETEM) experiments require specimen heating holders to study material behavior in gaseous environments at elevated temperatures. In order to extract meaningful kinetic parameters, such as activation energies, it is essential to have a direct and accurate measurement of local sample temperature. This is particularly important if the sample temperature might fluctuate, for example when room temperature gases are introduced to the sample area. Using selected-area diffraction (SAD) in an ETEM, the lattice parameter of Ag nanoparticles was measured as a function of the temperature and pressure of hydrogen gas to provide a calibration of the local sample temperature. SAD permits measurement of temperature to an accuracy of ±30°C using Ag lattice expansion. Gas introduction can cause sample cooling of several hundred degrees celsius for gas pressures achievable in the ETEM.


2017 ◽  
Vol 23 (4) ◽  
pp. 741-750 ◽  
Author(s):  
Sibylle Schilling ◽  
Arne Janssen ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke

AbstractThe capability to perform liquid in situ transmission electron microscopy (TEM) experiments provides an unprecedented opportunity to examine the real-time processes of physical and chemical/electrochemical reactions during the interaction between metal surfaces and liquid environments. This work describes the requisite steps to make the technique fully analytical, from sample preparation, through modifications of the electrodes, characterization of electrolytes, and finally to electrochemical corrosion experiments comparing in situ TEM to conventional bulk cell and microcell configurations.


2012 ◽  
Vol 18 (S2) ◽  
pp. 1114-1115 ◽  
Author(s):  
H. Zandbergen

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.


1985 ◽  
Vol 62 ◽  
Author(s):  
M. A. Parker ◽  
T. W. Sigmon ◽  
R. Sinclair

ABSTRACTA technique has been developed which employs high resolution transmission electron microscopy (HRTEM) for the observation of the atomic mechanisms associated with solid state phase transformation as they occur at elevated temperatures. It consists of the annealing in-situ of cross-section transmission electron microscopy (TEM) specimens that have been favorably oriented for lattice fringe imaging and the video-recording of dynamic events as they occur in real-time. By means of this technique, we report the first video-recorded lattice images of crystallographic defect motion in silicon, viz. the motion of dislocations and stacking faults, as well as the first such images of the atomic mechanisms responsible for the amorphous to crystalline (a-c) phase transformation, viz. heterogeneous nucleation of crystal nuclei, coalescence of crystal nuclei by co-operative atomic processes, ledge motion at the growth interface, and normal growth in silicon. This technique holds great potential for the elucidation of the atomic mechanisms involved in reaction kinetics in the solid state.


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