On the Microstructure of the Epoxy/Adherend Interphase

1995 ◽  
Vol 385 ◽  
Author(s):  
M. Libera ◽  
W. Zukas ◽  
S. Wentworth ◽  
A. Patel
Keyword(s):  
Dark Field ◽  
Interfacial Stress ◽  
Structural Variations ◽  
Anodized Aluminum ◽  
Scanning Calorimetry ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Adequate Understanding ◽  
Annular Dark Field ◽  
Aluminum Surfaces

ABSTRACTIt is now recognized that there is a region at the epoxy/adherend interface known as the interphase whose chemistry and structure are different from those of bulk epoxy. There is, however, no adequate understanding of its microstructure. This paper describes differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) studies of the interphase between an aromatic amine cured epoxy and alumina/oxidized-aluminum surfaces. DSC results show dramatic differences in resin-cure behavior in the presence of particulate alumina. TEM results on microtomed cross-sectional specimens of anodized aluminum wire embedded in epoxy show regions of incomplete epoxy infiltration and interfacial stress. RuO4 staining combined with high-angle annular-dark-field STEM imaging indicates that there are structural variations within the bulk epoxy at lengths of ∼10–30nm. The magnitude of these fluctuations decreases in the near the adherend interface, and there is a simultaneous variation in the average epoxy structure. A plausible interpretation of these observations is that the interphase region suffers a variation in curing-agent concentration of unknown magnitude and there is a higher concentration of homopolymerized epoxy there relative to the bulk.

Design of a new objective lens for an HB-501A STEM

1991 ◽  
Vol 49 ◽  
pp. 416-417
Author(s):  
Earl J. Kirkland ◽  
Robert J. Keyse
Keyword(s):  
High Resolution ◽  
Spherical Aberration ◽  
Scanning Transmission Electron Microscope ◽  
Dark Field ◽  
Objective Lens ◽  
Specimen Holder ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
High Resolution Microscopy

An ultra-high resolution pole piece with a coefficient of spherical aberration Cs=0.7mm. was previously designed for a Vacuum Generators HB-501A Scanning Transmission Electron Microscope (STEM). This lens was used to produce bright field (BF) and annular dark field (ADF) images of (111) silicon with a lattice spacing of 1.92 Å. In this microscope the specimen must be loaded into the lens through the top bore (or exit bore, electrons traveling from the bottom to the top). Thus the top bore must be rather large to accommodate the specimen holder. Unfortunately, a large bore is not ideal for producing low aberrations. The old lens was thus highly asymmetrical, with an upper bore of 8.0mm. Even with this large upper bore it has not been possible to produce a tilting stage, which hampers high resolution microscopy.

Characterization of reactive phase formation in sputter-deposited Ni/Al multilayer thin films using TEM

1996 ◽  
Vol 54 ◽  
pp. 1000-1001
Author(s):  
G. Lucadamo ◽  
K. Barmak ◽  
C. Michaelsen
Keyword(s):  
Thin Films ◽  
Phase Formation ◽  
Dark Field ◽  
Nickel Layer ◽  
Multilayer Thin Films ◽  
Cross Sectional ◽  
Dark Field Imaging ◽  
Transmission Electron ◽  
Sputter Deposited ◽  
Constant Heating

The subject of reactive phase formation in multilayer thin films of varying periodicity has stimulated much research over the past few years. Recent studies have sought to understand the reactions that occur during the annealing of Ni/Al multilayers. Dark field imaging from transmission electron microscopy (TEM) studies in conjunction with in situ x-ray diffraction measurements, and calorimetry experiments (isothermal and constant heating rate), have yielded new insights into the sequence of phases that occur during annealing and the evolution of their microstructure.In this paper we report on reactive phase formation in sputter-deposited lNi:3Al multilayer thin films with a periodicity A (the combined thickness of an aluminum and nickel layer) from 2.5 to 320 nm. A cross-sectional TEM micrograph of an as-deposited film with a periodicity of 10 nm is shown in figure 1. This image shows diffraction contrast from the Ni grains and occasionally from the Al grains in their respective layers.

scholarly journals Effect of Multiple Reflows on the Interfacial Reactions and Mechanical Properties of an Sn-0.5Cu-Al(Si) Solder and a Cu Substrate

Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2367
Author(s):  
Junhyuk Son ◽  
Dong-Yurl Yu ◽  
Yun-Chan Kim ◽  
Shin-Il Kim ◽  
Min-Su Kim ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
High Heat ◽  
Interfacial Reactions ◽  
Future Application ◽  
Scanning Calorimetry ◽  
Cross Sectional ◽  
Automotive Electronic ◽  
Transmission Electron ◽  
Si Content ◽  
Lead Free Solders

In this study, the interfacial reactions and mechanical properties of solder joints after multiple reflows were observed to evaluate the applicability of the developed materials for high-temperature soldering for automotive electronic components. The microstructural changes and mechanical properties of Sn-Cu solders regarding Al(Si) addition and the number of reflows were investigated to determine their reliability under high heat and strong vibrations. Using differential scanning calorimetry, the melting points were measured to be approximately 227, 230, and 231 °C for the SC07 solder, SC-0.01Al(Si), and SC-0.03Al(Si), respectively. The cross-sectional analysis results showed that the total intermetallic compounds (IMCs) of the SC-0.03Al(Si) solder grew the least after the as-reflow, as well as after 10 reflows. Electron probe microanalysis and transmission electron microscopy revealed that the Al-Cu and Cu-Al-Sn IMCs were present inside the solders, and their amounts increased with increasing Al(Si) content. In addition, the Cu6Sn5 IMCs inside the solder became more finely distributed with increasing Al(Si) content. The Sn-0.5Cu-0.03Al(Si) solder exhibited the highest shear strength at the beginning and after 10 reflows, and ductile fracturing was observed in all three solders. This study will facilitate the future application of lead-free solders, such as an Sn-Cu-Al(Si) solder, in automotive electrical components.

Atomic-scale structural and compositional analyses of Ruddlesden-Popper planar faults in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics

2009 ◽  
Vol 24 (8) ◽  
pp. 2596-2604 ◽  
Author(s):  
Sašo Šturm ◽  
Makoto Shiojiri ◽  
Miran Čeh
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Dark Field ◽  
Atomic Scale ◽  
Transmission Electron ◽  
Initial Stage ◽  
Final Microstructure ◽  
Scanning Transmission ◽  
The Matrix ◽  
Annular Dark Field

The microstructure in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics is strongly affected by the formation of Ruddlesden-Popper fault–rich (RP fault) lamellae, which are coherently intergrown with the matrix of the perovskite grains. We studied the structure and chemistry of RP faults by applying quantitative high-resolution transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy analyses. We showed that the Sr2+ and Ca2+ dopant ions form RP faults during the initial stage of sintering. The final microstructure showed preferentially grown RP fault lamellae embedded in the central part of the anisotropic perovskite grains. In contrast, the dopant Ba2+ ions preferably substituted for Sr2+ in the SrTiO3 matrix by forming a BaxSr1−xTiO3 solid solution. The surplus of Sr2+ ions was compensated structurally in the later stages of sintering by the formation of SrO-rich RP faults. The resulting microstructure showed RP fault lamellae located at the surface of equiaxed BaxSr1-xTiO3 perovskite grains.

scholarly journals Exploring the Capability of HAADF-STEM Techniques to Characterize Graphene Distribution in Nanocomposites by Simulations

2018 ◽  
Vol 2018 ◽  
pp. 1-12
Author(s):  
N. Baladés ◽  
D. L. Sales ◽  
M. Herrera ◽  
A. M. Raya ◽  
J. C. Hernández-Garrido ◽  
...  
Keyword(s):  
Electron Tomography ◽  
Carbon Matrix ◽  
Reconstruction Algorithm ◽  
Dark Field ◽  
Graphene Layers ◽  
Transmission Electron ◽  
Dispersion Degree ◽  
Scanning Transmission ◽  
The Matrix ◽  
Annular Dark Field

This paper explores the capability of scanning transmission electron microscopy (STEM) techniques in determining the dispersion degree of graphene layers within the carbon matrix by using simulated high-angle annular dark-field (HAADF) images. Results ensure that unmarked graphene layers are only detectable if their orientation is parallel to the microscope beam. Additionally, gold-marked graphene layers allow evaluating the dispersion degree in structural composites. Moreover, electron tomography has been demonstrated to provide truthfully 3D distribution of the graphene sheets inside the matrix when an appropriate reconstruction algorithm and 2D projections including channelling effect are used.

scholarly journals Transmission electron microscopy analysis of the crystallography of precipitates in Mg–Sn alloys aged at high temperatures

2014 ◽  
Vol 47 (5) ◽  
pp. 1729-1735 ◽  
Author(s):  
Xin Nie ◽  
Yimin Guan ◽  
Dongshan Zhao ◽  
Yu Liu ◽  
Jianian Gui ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Three Dimensional ◽  
Dark Field ◽  
Peak Hardness ◽  
Invariant Line ◽  
Orientation Relationships ◽  
Transmission Electron Microscopy Analysis ◽  
Transmission Electron ◽  
Annular Dark Field

The crystallographic orientation relationships (ORs) of precipitated β-Mg2Sn particles in Mg–9.76 wt% Sn alloy aged at 573 K for 5 h, corresponding to its peak hardness, were investigated by advanced transmission electron microscopy (TEM). OR-3 of (110)β//(0001)αand [\overline 111]β//[1\overline 210]αand OR-4 of (110)β//(0001)αand [001]β//[2\overline 1\overline 10]αare the key ORs of β-Mg2Sn particles in the alloy. The proportions of β-Mg2Sn particles exhibiting OR-3 and OR-4 were determined as 75.1 and 24.3%, respectively. Crystallographic factors determined the predominance of OR-3 in the precipitated β-Mg2Sn particles. This mechanism was analyzed by a three-dimensional invariant line model constructed using a transformation matrix in reciprocal space. Models of the interface of precipitated β-Mg2Sn and the α-Mg matrix were constructedviahigh-resolution TEM and atomic resolution high-angle annular dark-field scanning TEM.

scholarly journals Ru Catalyst Encapsulated into the Pores of MIL-101 MOF: Direct Visualization by TEM

Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4531
Author(s):  
Maria Meledina ◽  
Geert Watson ◽  
Alexander Meledin ◽  
Pascal Van Der Voort ◽  
Joachim Mayer ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Scanning Transmission Electron Microscopy ◽  
Dark Field ◽  
Catalyst Nanoparticles ◽  
Ru Catalyst ◽  
Ru Nanoparticles ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field

Ru catalyst nanoparticles were encapsulated into the pores of a Cr-based metal-organic framework (MOF)—MIL-101. The obtained material, as well as the non-loaded MIL-101, were investigated down to the atomic scale by annular dark-field scanning transmission electron microscopy using low dose conditions and fast image acquisition. The results directly show that the used wet chemistry loading approach is well-fitted for the accurate embedding of the individual catalyst nanoparticles into the cages of the MIL-101. The MIL-101 host material remains crystalline after the loading procedure, and the encapsulated Ru nanoparticles have a metallic nature. Annular dark field scanning transmission electron microscopy, combined with EDX mapping, is a perfect tool to directly characterize both the embedded nanoparticles and the loaded nanoscale MOFs. The resulting nanostructure of the material is promising because the Ru nanoparticles hosted in the MIL-101 pores are prevented from agglomeration—the stability and lifetime of the catalyst could be improved.

HREM and HAADF Studies of Precipitates in the Mg-Y-Nd Alloy System

2007 ◽  
Vol 561-565 ◽  
pp. 275-278
Author(s):  
Wei Sun ◽  
Li Sun ◽  
Lin Lin Liu ◽  
Ze Zhang
Keyword(s):  
Structural Model ◽  
Imaging Technique ◽  
Dark Field Image ◽  
Alloy System ◽  
Dark Field ◽  
Orthorhombic Unit Cell ◽  
Characteristic Distribution ◽  
Transmission Electron ◽  
Annular Dark Field ◽  
Image Technique

By means of high resolution transmission electron microscopy (HREM) and high-angle annular dark-field image technique (HAADF), morphological, structural and compositional characteristics of the precipitates in the Mg-4Y-3Nd alloy aged at 200°C for different periods of time have been studied. On the basis of HREM observations, an atomic structural model for the β’-precipitate with an orthorhombic unit cell has been proposed. The characteristic distribution of the precipitates which are rich in rare-earth elements (Y, Nd) has been clearly revealed by the HAADF imaging technique.

scholarly journals Synthesis of nickel/gallium nanoalloys using a dual-source approach in 1-alkyl-3-methylimidazole ionic liquids

2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dual Source ◽  
Induced Decomposition

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.

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