Transmission electron microscopy analyses of complex ceramics

Author(s):  
T. Shaw

Many potentially useful ceramic materials have complex structures which are difficult to determine using x-ray analysis alone. By the use of contemporary transmission electron microscopy-techniques such as lattice fringe imaging and contrast experiments much information can be obtained about such structures greatly simplifying structure determination. It has already been demonstrated that images of “open” structures bearing a one to one correspondence with the projected structure can be obtained. However, in many commercially important ceramics atoms or atom concentrations are two closely spaced to be resolved directly by current microscopes. In this presentation examples are shown of the type of structural information that is obtainable from such “close packed” structures using transmission electron microscopy, two examples being given below.In Fig. 1(a) a two dimensional fringe image of a region of a 15 R polytype from the Be-Si-N system is shown on the left. It can be seen from this image that the structure is made up of three identical blocks of five close packed planes each related by a translation of 1/3[100] giving a repeat stacking in the close packed [001] direction of fifteen close packed layers.

2009 ◽  
Vol 64 (8) ◽  
pp. 922-928 ◽  
Author(s):  
Manuel Christian Schaloske ◽  
Hansjürgen Mattausch ◽  
Viola Duppel ◽  
Lorenz Kienle ◽  
Arndt Simon

The compounds Pr6(C2)Br10, Pr10(C2)2Br15 and Pr14(C2)3Br20 were prepared from PrBr3 and the appropriate amounts of Pr and C and characterized by X-ray structure analyses of single crystals. All three compounds crystallize in space group P1 with lattice parameters a = 7.571(2), b = 9.004(2), c = 9.062(2) Å ,α = 108.57(3), β = 97.77(3), γ = 106.28(3)◦ for Pr6(C2)Br10; a = 9.098(2), b = 10.127(2), c = 10.965(2) A° , α = 70.38(3), β = 66.31(3), γ = 70.84(3)◦ for Pr10(C2)2Br15; a = 9.054(2), b = 10.935(2), c = 13.352(3) Å , α = 86.27(3), β = 72.57(3), γ = 66.88(3)◦ for Pr14(C2)3Br20. They are members of a general series Ln4n+2(C2)nBr5n+5 and isostructural with the corresponding iodides known for Ln = La, Ce, Pr. Pr6(C2)Br10 was further characterized via transmission electron microscopy techniques


2018 ◽  
Vol 4 (4) ◽  
pp. 68 ◽  
Author(s):  
Karolina Jurkiewicz ◽  
Mirosława Pawlyta ◽  
Andrzej Burian

Transmission electron microscopy and neutron or X-ray diffraction are powerful techniques available today for characterization of the structure of various carbon materials at nano and atomic levels. They provide complementary information but each one has advantages and limitations. Powder X-ray or neutron diffraction measurements provide structural information representative for the whole volume of a material under probe but features of singular nano-objects cannot be identified. Transmission electron microscopy, in turn, is able to probe single nanoscale objects. In this review, it is demonstrated how transmission electron microscopy and powder X-ray and neutron diffraction methods complement each other by providing consistent structural models for different types of carbons such as carbon blacks, glass-like carbons, graphene, nanotubes, nanodiamonds, and nanoonions.


2014 ◽  
Vol 2 (29) ◽  
pp. 11209-11221 ◽  
Author(s):  
Tashi Parsons-Moss ◽  
Jinxiu Wang ◽  
Stephen Jones ◽  
Erin May ◽  
Daniel Olive ◽  
...  

Batch, X-ray absorption spectroscopy, and transmission electron microscopy techniques revealed oxidized and pristine OMCs as high-capacity plutonium adsorbents, employing different mechanisms.


Polymers ◽  
2018 ◽  
Vol 10 (8) ◽  
pp. 865 ◽  
Author(s):  
Ewa Serwicka ◽  
Małgorzata Zimowska ◽  
Dorota Duraczyńska ◽  
Bogna Napruszewska ◽  
Małgorzata Nattich-Rak ◽  
...  

The effect of synthesis parameters on the physicochemical properties of clay/ polydiallyldimethylammonium (PDDA)/Ru composites and their applicability in hydrogenation of 2-butanone under very mild conditions (room temperature, atmospheric pressure, and aqueous solution) was studied. Three synthetic procedures were employed, differing in the order of addition of components and the stage at which metallic Ru species were generated. The materials were characterized with XRD (X-ray diffraction), XRF (X-ray fluorescence), EDS (energy-dispersive spectroscopy), AFM (atomic force microscopy), TEM/HRTEM (transmission electron microscopy/high resolution transmission electron microscopy), and TG/DSC (thermal gravimetry/differential scanning microscopy techniques. The study revealed that the method of composite preparation affects its structural and thermal properties, and controls the distribution and size of Ru particles. All catalysts are active in hydrogenation of 2-butanone. For best catalytic performance (100% conversion within 30 min) both the size of Ru particles and the load of polymer had to be optimized. Superior catalytic properties were obtained over the composite with intermediate crystal size and intermediate PDDA load, prepared by generation of metallic Ru species in the polymer solution prior to intercalation. This method offers an easy way of controlling the crystal size by modification of Ru/PDDA ratio.


Author(s):  
G. Thomas

Over the past two decades tremendous progress has been made in the use of advanced transmission electron microscopy techniques to solve complex materials problems. This is especially true in the case of inorganic materials, such as multicomponent metal oxides. The inherent complexity of the crystal structure and microstructure of these ceramic materials as well as the interdependence of the final properties on microstructure and processing mean that detailed characterization of the effect of processing variables on the structure and microstructure is imperative. Electron microscopy has become firmly established as a powerful tool to explore the structure and microstructure of these materials. Due to the various types of interactions of electrons with materials, the electron microscope is unique in that it can provide morphological, structural, compositional and in the case of materials such as ferroelectrics information on the domain and domain wall configurations. This is illustrated and summarized in Fig. 1. In this review, some typical examples of the applications of advanced transmission electron microscopy techniques to solving problems in ferroelectric materials will be discussed.


2020 ◽  
Vol 1 (1) ◽  
Author(s):  
Machteld E. Kamminga ◽  
Maria Batuk ◽  
Joke Hadermann ◽  
Simon J. Clarke

Abstract Topological superconductivity is of great contemporary interest and has been proposed in doped Bi2Se3, in which electron-donating atoms such as Cu, Sr or Nb have been intercalated into the Bi2Se3 structure. For NbxBi2Se3, with Tc ~ 3 K, it is assumed in the literature that Nb is inserted in the van der Waals gap. However, in this work an alternative origin for the superconductivity in Nb-doped Bi2Se3 is established. In contrast to previous reports, it is deduced that Nb intercalation in Bi2Se3 does not take place. Instead, the superconducting behaviour in samples of nominal composition NbxBi2Se3 results from the (BiSe)1.10NbSe2 misfit phase that is present in the sample as an impurity phase for small x (0.01 ≤ x ≤ 0.10) and as a main phase for large x (x = 0.50). The structure of this misfit phase is studied in detail using a combination of X-ray diffraction and transmission electron microscopy techniques.


Author(s):  
S. Fujishiro

The mechanical properties of three titanium alloys (Ti-7Mo-3Al, Ti-7Mo- 3Cu and Ti-7Mo-3Ta) were evaluated as function of: 1) Solutionizing in the beta field and aging, 2) Thermal Mechanical Processing in the beta field and aging, 3) Solutionizing in the alpha + beta field and aging. The samples were isothermally aged in the temperature range 300° to 700*C for 4 to 24 hours, followed by a water quench. Transmission electron microscopy and X-ray method were used to identify the phase formed. All three alloys solutionized at 1050°C (beta field) transformed to martensitic alpha (alpha prime) upon being water quenched. Despite this heavily strained alpha prime, which is characterized by microtwins the tensile strength of the as-quenched alloys is relatively low and the elongation is as high as 30%.


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