TEM/STEM Characterization of Rapidly Solidified Aluminum Alloys

Author(s):  
R. J. Kar ◽  
T. P. McHale ◽  
R. T. Kessler

Low-density and high strength-type rapidly solidified (RST) aluminum alloys offer promise for structural aerospace applications. At Northrop, as part of a continuing program to establish structure-property relationships in advanced materials, detailed transmission electron microscopy (TEM)/scanning transmission electron microscopy (STEM) of candidate RST aluminum-lithium (Al-Li) and high strength (7XXX-type) aluminum-copper-magnesium-zinc (Al-Cu-Mg-Zn) alloys is routinely performed. This paper describes typical microstructural features that we have observed in these alloys.Figure 1 illustrates the microstructure of an inert-gas atomized RST Al-Li-Cu-Mg-Zr alloy. Frequently the grain boundaries are decorated with continuous or semi-continuous stringers of oxide that are relatively opaque to the incident electron beam. These have been identified to be Al-,Mg-, and Li- containing oxides present on powder particle surfaces prior to consolidation, and which have not been adequately broken up and dispersed by post-consolidation processing. The microstructures of these alloys are generally characterized by unrecystallized grains and equiaxed sub-grains pinned by fine (0.2μm) precipitates. These have been identified to be Al3Zr dispersoids using a combination of selected area diffraction/energy-dispersive x-ray (SAD/EDX) methods.

2021 ◽  
Vol 56 (9) ◽  
pp. 5309-5320
Author(s):  
Khalid Hattar ◽  
Katherine L. Jungjohann

Abstract Multimodal in-situ experiments are the wave of the future, as this approach will permit multispectral data collection and analysis during real-time nanoscale observation. In contrast, the evolution of technique development in the electron microscopy field has generally trended toward specialization and subsequent bifurcation into more and more niche instruments, creating a challenge for reintegration and backward compatibility for in-situ experiments on state-of-the-art microscopes. We do not believe this to be a requirement in the field; therefore, we propose an adaptive instrument that is designed to allow nearly simultaneous collection of data from aberration-corrected transmission electron microscopy (TEM), probe-corrected scanning transmission electron microscopy, ultrafast TEM, and dynamic TEM with a flexible in-situ testing chamber, where the entire instrument can be modified as future technologies are developed. The value would be to obtain a holistic understanding of the underlying physics and chemistry of the process-structure–property relationships in materials exposed to controlled extreme environments. Such a tool would permit the ability to explore, in-situ, the active reaction mechanisms in a controlled manner emulating those of real-world applications with nanometer and nanosecond resolution. If such a powerful tool is developed, it has the potential to revolutionize our materials understanding of nanoscale mechanisms and transients. Graphical Abstract


Crystals ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 878
Author(s):  
Hasti Vahidi ◽  
Komal Syed ◽  
Huiming Guo ◽  
Xin Wang ◽  
Jenna Laurice Wardini ◽  
...  

Interfaces such as grain boundaries (GBs) and heterointerfaces (HIs) are known to play a crucial role in structure-property relationships of polycrystalline materials. While several methods have been used to characterize such interfaces, advanced transmission electron microscopy (TEM) and scanning TEM (STEM) techniques have proven to be uniquely powerful tools, enabling quantification of atomic structure, electronic structure, chemistry, order/disorder, and point defect distributions below the atomic scale. This review focuses on recent progress in characterization of polycrystalline oxide interfaces using S/TEM techniques including imaging, analytical spectroscopies such as energy dispersive X-ray spectroscopy (EDXS) and electron energy-loss spectroscopy (EELS) and scanning diffraction methods such as precession electron nano diffraction (PEND) and 4D-STEM. First, a brief introduction to interfaces, GBs, HIs, and relevant techniques is given. Then, experimental studies which directly correlate GB/HI S/TEM characterization with measured properties of polycrystalline oxides are presented to both strengthen our understanding of these interfaces, and to demonstrate the instrumental capabilities available in the S/TEM. Finally, existing challenges and future development opportunities are discussed. In summary, this article is prepared as a guide for scientists and engineers interested in learning about, and/or using advanced S/TEM techniques to characterize interfaces in polycrystalline materials, particularly ceramic oxides.


Author(s):  
J. M. Cowley

The comparison of scanning transmission electron microscopy (STEM) with conventional transmission electron microscopy (CTEM) can best be made by means of the Reciprocity Theorem of wave optics. In Fig. 1 the intensity measured at a point A’ in the CTEM image due to emission from a point B’ in the electron source is equated to the intensity at a point of the detector, B, due to emission from a point A In the source In the STEM. On this basis it can be demonstrated that contrast effects In the two types of instrument will be similar. The reciprocity relationship can be carried further to include the Instrument design and experimental procedures required to obtain particular types of information. For any. mode of operation providing particular information with one type of microscope, the analagous type of operation giving the same information can be postulated for the other type of microscope. Then the choice between the two types of instrument depends on the practical convenience for obtaining the required Information.


Author(s):  
Kenichi Takaya

Mast cell and basophil granules of the vertebrate contain heparin or related sulfated proteoglycans. Histamine is also present in mammalian mast cells and basophils. However, no histamine is detected in mast cell granules of the amphibian or fish, while it is shown in those of reptiles and birds A quantitative x-ray microanalysis of mast cell granules of fresh frozen dried ultrathin sections of the tongue of Wistar rats and tree frogs disclosed high concentrations of sulfur in rat mast cell granules and those of sulfur and magnesium in the tree frog granules. Their concentrations in tree frog mast cell granules were closely correlated (r=0.94).Fresh frozen dried ultrathin sections and fresh air-dried prints of the tree frog tongue and spleen and young red-eared turtle (ca. 6 g) spleen and heart blood were examined by a quantitative energy-dispersive x-ray microanalysis (X-650, Kevex-7000) for the element constituents of the granules of mast cells and basophils. The specimens were observed by transmission electron microscopy (TEM) (80-200 kV) and followed by scanning transmission electron microscopy (STEM) under an analytical electron microscope (X-650) at an acceleration voltage of 40 kV and a specimen current of 0.2 nA. A spot analysis was performed in a STEM mode for 100 s at a specimen current of 2 nA on the mast cell and basophil granules and other areas of the cells. Histamine was examined by the o-phthalaldehyde method.


Author(s):  
F. Khoury ◽  
L. H. Bolz

The lateral growth habits and non-planar conformations of polyethylene crystals grown from dilute solutions (<0.1% wt./vol.) are known to vary depending on the crystallization temperature.1-3 With the notable exception of a study by Keith2, most previous studies have been limited to crystals grown at <95°C. The trend in the change of the lateral growth habit of the crystals with increasing crystallization temperature (other factors remaining equal, i.e. polymer mol. wt. and concentration, solvent) is illustrated in Fig.l. The lateral growth faces in the lozenge shaped type of crystal (Fig.la) which is formed at lower temperatures are {110}. Crystals formed at higher temperatures exhibit 'truncated' profiles (Figs. lb,c) and are bound laterally by (110) and (200} growth faces. In addition, the shape of the latter crystals is all the more truncated (Fig.lc), and hence all the more elongated parallel to the b-axis, the higher the crystallization temperature.


Author(s):  
Dongmei Meng ◽  
Laura Buck ◽  
James Cargo

Abstract Cu needs a higher level of ultrasound combined with bonding force to be bonded to the Al pad properly, not just because Cu is harder than Au, but it is also harder to initiate intermetallic compounds (IMC) formation during bonding. This increases the chances of damaging the metal/low k stack under the bondpad. This paper presents a fundamental study of IMC as well as one example of a failure mode of Cu/Al bonded devices, all based on detailed analysis using scanning electron microscopy, scanning transmission electron microscopy, energy dispersive spectrometers, and transmission electron microscopy. It presents a case study showing a corrosion mechanism of Cu/Al ballbond after 168hr UHAST stress. It is observed that all Cu9Al4 was consumed, while very little copper aluminide remained after 168 hours of UHAST stressing.


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