The effect of small additions of Cu on precipitation in Al-Mg-Si alloys

Author(s):  
M. Tamizifar ◽  
G. Cliff ◽  
R.W. Devenish ◽  
G.W. Lorimer

Small additions of copper, <1 wt%, have a pronounced effect on the ageing response of Al-Mg-Si alloys. The object of the present investigation was to study the effect of additions of copper up to 0.5 wt% on the ageing response of a series of Al-Mg-Si alloys and to use high resolution analytical electron microscopy to determine the composition of the age hardening precipitates.The composition of the alloys investigated is given in Table 1. The alloys were heat treated in an argon atmosphere for 30m, water quenched and immediately aged either at 180°C for 15 h or given a duplex treatment of 180°C for 15 h followed by 350°C for 2 h2. The double-ageing treatment was similar to that carried out by Dumolt et al. Analyses of the precipitation were carried out with a HB 501 Scanning Transmission Electron Microscope. X-ray peak integrals were converted into weight fractions using the ratio technique of Cliff and Lorimer.

2014 ◽  
Vol 20 (2) ◽  
pp. 323-329 ◽  
Author(s):  
Nestor J. Zaluzec ◽  
M. Grace Burke ◽  
Sarah J. Haigh ◽  
Matthew A. Kulzick

AbstractThe use of analytical spectroscopies during scanning/transmission electron microscope (S/TEM) investigations of micro- and nano-scale structures has become a routine technique in the arsenal of tools available to today’s materials researchers. Essential to implementation and successful application of spectroscopy to characterization is the integration of numerous technologies, which include electron optics, specimen holders, and associated detectors. While this combination has been achieved in many instrument configurations, the integration of X-ray energy-dispersive spectroscopy and in situ liquid environmental cells in the S/TEM has to date been elusive. In this work we present the successful incorporation/modifications to a system that achieves this functionality for analytical electron microscopy.


Author(s):  
Sooho Kim

Automotive catalysts have a general loss of activity during aging, basically due to two principal deactivation mechanisms. One of them is thermally induced “sintering,” which results in catalytic surface area reduction. The other is chemically induced “poisoning,” which in part causes blockage of active metal sites. The conventional bulk techniques have indicated that various catalyst functions were affected differently by poisons and thermal damage; however, they generally did not provide detailed descriptions of the mechanisms of deactivation. Only analytical electron microscopy (AEM) can provide microchemical and microstructural information to gain a more thorough and fundamental understanding of catalytic deactivation.Fresh and vehicle-aged commercial automotive catalysts containing Pt, Pd, and Rh on alumina supports were prepared for AEM by a microtomy technique, which retains the spatial integrity of the catalyst pellet with uniform thickness. Then these AEM specimens were characterized in a transmission electron microscope (TEM) and in a dedicated scanning transmission electron microscope (STEM).


1997 ◽  
Vol 12 (9) ◽  
pp. 2438-2446 ◽  
Author(s):  
M. Čeh ◽  
H. Gu ◽  
H. Müllejans ◽  
A. Rečnik

Oxide-rich planar faults within a perovskite matrix are the prevailing type of extended defects in polycrystalline SrO-doped CaTiO3. These defects form, depending on the temperature of sintering, random networks, or ordered structures. The chemistry of the polytypoid, the isolated planar faults, and the perovskite phase have been studied by spatially resolved electron energy-loss and energy-dispersive x-ray spectroscopies using a dedicated scanning transmission electron microscope. We have found that Sr ions from SrO additions preferably substitute Ca in the CaTiO3 lattice, thus forming a solid solution (Ca1–xSrx)TiO3. The surplus of Ca ions forms single and ordered CaO-rich planar faults in the host (Ca1–xSrx)TiO3 phase. Whereas the excess Ca segregates in a form of single planar faults at lower temperatures, it forms a stable polytypoidic phase at higher temperatures. For materials having up to 25 mol% of SrO additions, this phase has (Ca1–xSrx)4Ti3O10 composition, comprising a sequence of CaO faults followed by three (Ca1–xSrx)TiO3 perovskite layers. Analytical electron microscopy revealed that the composition of the single planar faults, formed at lower temperatures, is identical to that of polytypoids, which are stable at higher sintering temperatures.


Author(s):  
J. R. Michael ◽  
K. A. Taylor

Although copper is considered an incidental or trace element in many commercial steels, some grades contain up to 1-2 wt.% Cu for precipitation strengthening. Previous electron microscopy and atom-probe/field-ion microscopy (AP/FIM) studies indicate that the precipitation of copper from ferrite proceeds with the formation of Cu-rich bcc zones and the subsequent transformation of these zones to fcc copper particles. However, the similarity between the atomic scattering amplitudes for iron and copper and the small misfit between between Cu-rich particles and the ferrite matrix preclude the detection of small (<5 nm) Cu-rich particles by conventional transmission electron microscopy; such particles have been imaged directly only by FIM. Here results are presented whereby the Cu Kα x-ray signal was used in a dedicated scanning transmission electron microscope (STEM) to image small Cu-rich particles in a steel. The capability to detect these small particles is expected to be helpful in understanding the behavior of copper in steels during thermomechanical processing and heat treatment.


Clay Minerals ◽  
2001 ◽  
Vol 36 (3) ◽  
pp. 307-324 ◽  
Author(s):  
M. D. Ruiz Cruz

AbstractMixed-layered phyllosilicates with composition intermediate between mica and chlorite were identified in very low-grade metaclastites from the Malàguide Complex (Betic Cordilleras, Spain), and studied by X-ray diffraction, and transmission and analytical electron microscopy. They occur both as small grains in the rock matrix, and associated with muscovitechlorite stacks. Transmission electron microscope observations revealed a transition from chlorite to ordered 1:1 interstratifications through complex 1:2 and 1:3 interstratifications. Analytical electron microscopy data indicate a composition slightly different from the sum of discrete trioctahedral chlorite and dioctahedral mica. The types of layer transitions suggest that mixed-layer formation included two main processes: (1) the replacement of a brucite sheet by a cation sheet in the chlorite structure; and (2) the precipitation of mica-like layers between the chlorite layers. The strongest diffraction lines in oriented X-ray patterns are: 12.60 Å (002), 7.98 Å (003), 4.82 Å (005) and 3.48 Å (007).


2014 ◽  
Vol 20 (4) ◽  
pp. 1318-1326 ◽  
Author(s):  
Nestor J. Zaluzec

AbstractClosed form analytical equations used to calculate the collection solid angle of six common geometries of solid-state X-ray detectors in scanning and scanning/transmission analytical electron microscopy are presented. Using these formulae one can make realistic comparisons of the merits of the different detector geometries in modern electron column instruments. This work updates earlier formulations and adds new detector configurations.


Author(s):  
L. E. Thomas

Continuing evolution of energy-dispersive x-ray spectrometer (EDS) systems has greatly advanced x-ray detector performance in analytical electron microscopes. The latest detectors offer improved energy resolution, count rate performance, geometrical collection efficiency, durability, and efficiency for light and heavy elements. Innovative detector designs for transmission and scanning transmission electron microscopes (TEM/STEMs) include such features as liquid-nitrogen-free operation, in situ de-icing of the detector crystal, user cleanable windows, demountable windows, ultrahigh vacuum compatibility (including adaptations to allow microscope bakeouts without removing the detector), beam damage protection, and microscope interfaces with optimized collection geometries. Divergent design philosophies have produced a variety of systems with specialized features, and users may face hard choices in selecting the best detector for the job. The aim of this paper is to review the current state of EDS detector development and the importance of the performance improvements to TEM/STEM users.


Author(s):  
D. B. Williams

With the development of the scanning transmission electron microscope (STEM) the TEM was transformed into an analytical instrument capable of high resolution microanalysis and diffraction, as well as offering a broad range of imaging techniques. The combination of a < 10 nm electron probe and thin foil specimens permits analytical information to be gained from regions < 50 nm in diameter since beam spreading in thin specimens is of this order. This article will use specific examples to illustrate the possible applications of STEM in the study of materials, as well as the physical limitations of the analysis procedure which are only now being defined.


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