Strain Relaxation and In-Situ Observation of Voiding in Passivated Aluminum Alloy Lines.

1993 ◽  
Vol 308 ◽  
Author(s):  
Paul R. Besser ◽  
Thomas N. Marieb ◽  
John C. Bravman
Keyword(s):  
Strain Relaxation ◽  
Grazing Incidence ◽  
Scanning Transmission Electron Microscope ◽  
In Situ Observation ◽  
X Ray ◽  
Scanning Transmission ◽  
Length Width ◽  
Measured Strain ◽  
Ray Geometry

ABSTRACTStrain relaxation in passivated Al-0.5% Cu lines was measured using X-ray diffraction coupled with in-situ observation of the formation and growth of stress induced voids. Samples of 1 μm thick Al-0.5% Cu lines passivated with Si3N4 were heated to 380ºC, then cooled and held at 150ºC. During the test, principal strains along the length, width, and height of the line were determined using a grazing incidence x-ray geometry. From these measurements the hydrostatic strain in the metal was calculated and strain relaxation was observed. The thermal cycle was duplicated in a high voltage scanning transmission electron microscope equipped with a backscattered electron detector. The 1.25 μm wide lines were seen to have initial stress voids. Upon heating these voids reduced in size until no longer observable. Once the samples were cooled to 150ºC, voids reappeared and grew. The measured strain relaxation is discussed in terms of void and θ-phase (Al2Cu) formation.

Strain Relaxation and In-Situ Observation of Voiding in Passivated Aluminum alloy Lines

1993 ◽  
Vol 309 ◽  
Author(s):  
Paul R. Besser ◽  
Thomas N. Marieb ◽  
John C. Bravman
Keyword(s):  
Strain Relaxation ◽  
Grazing Incidence ◽  
Scanning Transmission Electron Microscope ◽  
In Situ Observation ◽  
X Ray ◽  
Scanning Transmission ◽  
Length Width ◽  
Measured Strain ◽  
Ray Geometry

AbstractStrain relaxation in passivated Al-0.5% Cu lines was measured using X-ray diffraction coupled with in-situ observation of the formation and growth of stress induced voids. Samples of 1 μm thick Al-0.5% Cu lines passivated with Si3N4 were heated to 380°C, then cooled and held at 150°C. During the test, principal strains along the length, width, and height of the line were determined using a grazing incidence x-ray geometry. From these measurements the hydrostatic strain in the metal was calculated and strain relaxation was observed. The thermal cycle was duplicated in a high voltage scanning transmission electron microscope equipped with a backscattered electron detector. The 1.25 μm wide lines were seen to have initial stress voids. Upon heating these voids reduced in size until no longer observable. Once the samples were cooled to 150°C, voids reappeared and grew. The measured strain relaxation is discussed in terms of void and θ-phase (Al2Cu) formation.

X-ray Energy-Dispersive Spectrometry During In Situ Liquid Cell Studies Using an Analytical Electron Microscope

2014 ◽  
Vol 20 (2) ◽  
pp. 323-329 ◽  
Author(s):  
Nestor J. Zaluzec ◽  
M. Grace Burke ◽  
Sarah J. Haigh ◽  
Matthew A. Kulzick
Keyword(s):  
Electron Microscope ◽  
Analytical Electron Microscopy ◽  
Scanning Transmission Electron Microscope ◽  
Energy Dispersive ◽  
X Ray ◽  
Transmission Electron ◽  
Analytical Electron ◽  
Scanning Transmission ◽  
Liquid Cell

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.

Amorphous Ni-Zr Phase Formation in Self-Supporting Thin-Film Lateral-Diffusion Couples

1985 ◽  
Vol 57 ◽  
Author(s):  
J. C. Barbour ◽  
J. W. Mayer
Keyword(s):  
Amorphous Phase ◽  
Amorphous Material ◽  
Lateral Diffusion ◽  
Scanning Transmission Electron Microscope ◽  
Vacuum Furnace ◽  
In Situ Observation ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Zr Alloy

AbstractThe formation of an amorphous Ni-Zr alloy, by heating to cause interdiffusion in the temperature range 250°C to 325°C, was demonstrated in a self-supporting lateral-diffusion couple. Micro-area diffraction in a scanning transmission electron microscope (STEM) indicates that microcrystalline ordering in the amorphous phase must be on a scale less than 5 nm. The samples were heated in a vacuum furnace to form the amorphous phase and later heated in the STEM for in situ observation of crystalline compoundformation. The amorphous to crystalline transformation occurs first in theZr-rich regions at 370°C. A crystalline phase begins to consume the Ni rich amorphous material, at 450° C; but at 325° C, the amorphous phase is stable up to 20.5 hours, even in the presence of crystalline compounds.

In-Situ Observation of The Initial Stages of Co (0001) Epitaxy on Pt (111) Using Grazing Incidence X-Ray Diffraction

1993 ◽  
Vol 312 ◽  
Author(s):  
James A. Bain ◽  
Bruce M. Clemens ◽  
Sean Brennan
Keyword(s):  
Early Stage ◽  
Stacking Faults ◽  
Grazing Incidence ◽  
In Situ Observation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Incoherent Interface ◽  
X Ray Scattering ◽  
Fault Density

AbstractThe heteropitaxial growth of (111) Pt on (0001) sapphire and of (0001) Co on (111) Pt on (0001) sapphire has been observed in-situ using grazing incidence x-ray scattering (GIXS). The in-plane lattice parameters of the Pt and Co phases have been measured as a function of film thickness in the regime from two monolayers to 200 monolayers, Relaxation of elastic strain with thickness has been quantified. X-ray reflections consistent with stacking faults in the Co films have been observed and monitored as a function of thickness, giving a measure of the stacking fault density. A distinct Co phase was observed at two monolayers of Co on a thick Pt layer, indicating an incoherent interface between the Co and Pt, even at this very early stage of deposition.

High-resolution x-ray imaging of small copper-rich precipitates in steels

1988 ◽  
Vol 46 ◽  
pp. 528-529
Author(s):  
J. R. Michael ◽  
K. A. Taylor
Keyword(s):  
Electron Microscopy ◽  
Thermomechanical Processing ◽  
Atom Probe ◽  
Ferrite Matrix ◽  
Scanning Transmission Electron Microscope ◽  
Probe Field ◽  
X Ray ◽  
Subsequent Transformation ◽  
Transmission Electron ◽  
Scanning Transmission

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.

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

1990 ◽  
Vol 48 (2) ◽  
pp. 442-443
Author(s):  
M. Tamizifar ◽  
G. Cliff ◽  
R.W. Devenish ◽  
G.W. Lorimer
Keyword(s):  
Electron Microscopy ◽  
Analytical Electron Microscopy ◽  
Scanning Transmission Electron Microscope ◽  
Argon Atmosphere ◽  
Age Hardening ◽  
X Ray ◽  
Transmission Electron ◽  
Heat Treated ◽  
Analytical Electron ◽  
Scanning Transmission

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.

High Spatial Resolution Compositional Analysis at Interfaces

1980 ◽  
Vol 38 ◽  
pp. 356-359
Author(s):  
John B. Vander Sande ◽  
Thomas F. Kelly ◽  
Douglas Imeson
Keyword(s):  
Electron Microscope ◽  
High Spatial Resolution ◽  
Compositional Analysis ◽  
Scanning Transmission Electron Microscope ◽  
Thin Specimen ◽  
X Ray ◽  
Volume Of Interest ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Electron Energy Loss

In the scanning transmission electron microscope (STEM) a fine probe of electrons is scanned across the thin specimen, or the probe is stationarily placed on a volume of interest, and various products of the electron-specimen interaction are then collected and used for image formation or microanalysis. The microanalysis modes usually employed in STEM include, but are not restricted to, energy dispersive X-ray analysis, electron energy loss spectroscopy, and microdiffraction.

scholarly journals In Situ Thermal-Stage Fitted-STEM Characterization of Spherical-Shaped Co/MoS2 Nanoparticles for Conversion of Heavy Crude Oils

Catalysts ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1239
Author(s):  
Manuel Ramos ◽  
Félix Galindo-Hernández ◽  
Brenda Torres ◽  
José Manuel Domínguez-Esquivel ◽  
Martin Heilmaier
Keyword(s):  
Molybdenum Disulfide ◽  
Sodium Molybdate ◽  
Interlayer Spacing ◽  
Scanning Transmission Electron Microscope ◽  
Interplanar Distance ◽  
Scanning Transmission ◽  
Heavy Crude ◽  
C 50 ◽  
Nano Catalysts

We report the thermal stability of spherically shaped cobalt-promoted molybdenum disulfide (Co/MoS2) nano-catalysts from in-situ heating under electron irradiation in the scanning transmission electron microscope (STEM) from room temperature to 550 °C ± 50 °C with aid of Fusion® holder (Protochip©, Inc.). The catalytic nanoparticles were synthesized via a hydrothermal method using sodium molybdate (Na2MoO4·2H2O) with thioacetamide (CH3CSNH2) and cobalt chloride (CoCl2) as promoter agent. The results indicate that the layered molybdenum disulfide structure with interplanar distance of ~0.62 nm remains stable even at temperatures of 550 °C, as observed in STEM mode. Subsequently, the samples were subjected to catalytic tests in a Robinson Mahoney Reactor using 30 g of Heavy Crude Oil (AGT-72) from the golden lane (Mexico’s east coast) at 50 atm using (ultrahigh purity) UHP hydrogen under 1000 rpm stirring at 350 °C for 8 h. It was found that there is no damage on the laminar stacking of Co/MoS2 with temperature, with interlayer spacing remaining at 0.62 nm; these sulfided catalytic materials led to aromatics rise of 22.65% and diminution of asphaltenes and resins by 15.87 and 3.53%, respectively.

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