Method and results of studying vapor deposition nucleation processes by in situ electron microscopy
In situ electron microscopy for studying vapor deposition nucleation processes
Poppa, H.↗
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In Situ Raman Microscopy of a Single Graphite Microflake Electrode in a Li(+)-containing Electrolyte
Highly detailed Raman spectra from a single KS-44 graphite microflake electrode as a function of the applied potential have been collected in situ using a Raman microscope and a sealed spectroelectrochemical cell isolated from the laboratory environment. Correlations were found between the Raman spectral features and the various Li(+) intercalation stages while recording in real time Raman spectra during a linear potential scan from 0.7 down ca. 0.0V vs Li/Li(+) at a rate of 0.1 mV/s in a 1M LiClO4 solution in a 1:l (by volume) ethylene carbonate (EC):diethyl carbonate (DEC) mixture. In particular, clearly defined isosbestic points were observed for data collected in the potential range where the transition between dilute phase 1 and phase 4 of lithiated graphite is known to occur, i.e. 0.157 < E < 0.215 vs Li/Li(+). Statistical analysis of the spectroscopic data within this region made it possible to determine independently the fraction of each of the two phases present as a function of potential without relying on coulometric information and then predict, based on the proposed stoichiometry for the transition, a spectrally-derived voltammetric feature.
Shi, Qing-Fang↗
Heterogeneous Nucleation of Bi and Ag on Amorphous Substrates (In Situ Electron Microscopy Studies)
Bi and Ag nucleation on evaporated substrates studied as function of substrate temperature and impinging flux using electron microscopy
ELECTRON MICROSCOPY↗
Microstructure-Sensitive Investigation of Fracture Using Acoustic Emission Coupled With Electron Microscopy
A novel technique using Scanning Electron Microscopy (SEM) in conjunction with Acoustic Emission (AE) monitoring is proposed to investigate microstructure-sensitive fatigue and fracture of metals. The coupling between quasi in situ microscopy with actual in situ nondestructive evaluation falls into the ICME framework and the idea of quantitative data-driven characterization of material behavior. To validate the use of AE monitoring inside the SEM chamber, Aluminum 2024-B sharp notch specimen were tested both inside and outside the microscope using a small scale mechanical testing device. Subsequently, the same type of specimen was tested inside the SEM chamber. Load data were correlated with both AE information and observations of microcracks around grain boundaries as well as secondary cracks, voids, and slip bands. The preliminary results are in excellent agreement with similar findings at the mesoscale. Extensions of the application of this novel technique are discussed.
Wisner, Brian↗
Australian Red Dune Sand: A Potential Martian Regolith Analog
To demonstrate the potential scientific and technical merits of in situ microscopy on Mars, we analyzed a possible Martian regolith analog - an acolian red dune sand from the central Australian desert (near Mt. Olga). This sand was chosen for its ubiquitous red coating and the desert environment in which is it found. Grains of this sand were analyzed using a variety of microanalytical techniques. A database of detailed studies of such terrestrial analogs would assist the study of geological and astrobiological specimens in future missions to Mars. Potential instrument concepts for in situ deployment on Mars include local electrode atom probe nanoanalysis (LEAP), vertical scanning white light interferometry (VSWLI), scanning electron microscopies, energy dispersive x-ray microanalysis (EDX), atomic force microscopy (AFM) and X-ray diffraction (XRD). While in situ deployment of these techniques is many years away, ground-based studies using these analytical techniques extend our understanding of the data obtained from instruments to be flown in the near future.
Kuhlman, K. R.↗
Morphology and capacity of a cadmium electrode - Studies on a simulated pore.
Conditions in a single pore of a battery plate were simulated by using a cadmium chip of millimeter dimensions covered with an electrolyte film of micron thickness. In situ microscopy was applied to study changes in the electrode morphology during charge and discharge. Passivation and increases in particle sizes due to precipitation and electrodeposition of dissolved cadmium species were found to cause profound loss in electrode capacity on repeated charge and discharge.
Will, F. G.↗
In situ transmission electron microscopy study on the epitaxial growth of CoSi2 on Si(111) at temperatures below 150 C
This paper reports an in situ transmission electron microscopy study on the epitaxial growth of CoSi2 on Si(111) from a 10-nm-thick amorphous mixture of Co and Si in the ratio 1:2, which was formed by codeposition of Co and Si near room temperature. Nuclei of CoSi2 are observed in the as-deposited film. These nuclei are epitaxial and extend through the whole film thickness. Upon annealing, these columnar epitaxial CoSi2 grains grow laterally at temperatures as low as 50 C. The kinetics of this lateral epitaxial growth was studied at temperatures between 50 and 150 C. The activation energy of the growth process is 0.8 + or - 0.1 eV.
Nieh, C. W.↗
Oxidation of metals and alloys in controlled atmospheres using in situ transmission electron microscopy and Auger spectrography
Single-crystalline thin films of copper were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of .005 Torr in situ in a high-resolution electron microscope. The specimens were prepared by epitaxial vapor deposition onto polished 100 and 110 faces of rocksalt and mounted in a hot stage inside an ultra-high-vacuum specimen chamber of the microscope. Large amounts of sulfur, carbon, and oxygen were detected by Auger electron spectroscopy on the surface of the as-received films and were removed in situ by ion-sputter etching immediately prior to the oxidation. The nucleation and growth characteristics of Cu2O on Cu were studied. Results show that neither stacking faults nor dislocations are associated with the Cu2O nucleation sites. The growth of Cu2O nuclei is linear with time. The experimental findings, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving (a) the formation of a surface-charge layer, (b) oxygen saturation in the metal and (c) nucleation, followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.
Rao, D. B.↗
An ultrahigh vacuum multipurpose specimen chamber with sample introduction system for in situ transmission electron microscopy investigations
A commercial transmission electron microscope (TEM), with flat-plate upper pole piece configuration of the objective lens, and top-entry specimen introduction was modified by introducing an ultrahigh vacuum (UHV) specimen chamber for in situ TEM experimentation. The pumping and design principles and special features of this UHV chamber, which makes it possible to obtain 5 x 10 to the -10th mbar pressure at the site of the specimen, while maintaining the airlock system that allows operation in the 10 to the -10th mbar range within 15 min after specimen change, are described. Design operating pressures and image quality (resolution of metal particles smaller than 1 nm in size) were achieved. Schematic drawings and design dimensions are included.
Heinemann, K.↗
In-Situ X-Ray Microscopy of Phase and Composition Distributions in Metal Alloys During Solidification
This research applies a state of the art X-ray Transmission Microscope, to image the solidification of metallic or semiconductor alloys in real-time. By employing a hard x-ray source with sub-micron dimensions, resolutions of up to 3 gm can be obtained with magnifications of over 800 X. Specimen growth conditions were optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid inter-face. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. Composition gradients within the specimen cause vafiations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). During this study, the growth of secondary phase fibers and lameilae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Keywords: x-ray, microscope, solidification, microfocus, real-time, microstructure
Kaukler, William F.↗
Structural characterization and gas reactions of small metal particles by high resolution in-situ TEM (Transmission Electron Microscopy) and TED (Transmission Electron Diffraction)
The detection and size analysis of small metal particles supported on amorphous substrates becomes increasingly difficult when the particle size approaches that of the phase contrast background structures of the support. An approach of digital image analysis, involving Fourier transformation of the original image, filtering, and image reconstruction was studied with respect to the likelihood of unambiguously detecting particles of less than 1 nm diameter on amorphous substrates from a single electron micrograph.
Heinemann, K.↗
Transmission Electron Microscopy of an In Situ Presolar Silicon Carbide Grain
We used a focused ion beam workstation to prepare ultra-thin sections of a presolar SiC grain. Our TEM studies indicate that the SiC formed by rapid vapor-phase condensation, trapping pre-existing graphite grains in random orientations. Additional information is contained in the original extended abstract.
Stroud, Rhonda M.↗
High Temperature Material Property Data and Challenges to Thermal Process Model Predictions and In-Situ/Ex-Situ Measurements for Metallic Additive Manufacturing
Understanding and predicting performance properties of parts produced by metallic additive manufacturing has improved significantly over the past decade; however, difficult to measure material properties and process outcomes continue to be challenges. The qualification or certification of aerospace parts require extensive measures to quantify variable part properties in order to buy down the risk of component failure. The variability, inherent to the additive manufacturing, process adds unwanted uncertainty in the production of load critical structural components. Process modeling has proven valuable in providing predictions and context for understanding outcomes of the additive manufacturing process; however, these physically informed process models require material properties at temperatures that are difficult to measure and rarely available. Further, calibrating or validating such models is difficult because the process itself is challenging to measure. This talk will explore some of the challenges resulting from difficult to acquire input data by relating thermal process model predictions to in-situ and ex-situ optical microscopy measurements.
Process Model↗
In situ sputter cleaning of thin film metal substrates for UHV-TEM corrosion studies.
A prerequisite for conducting valid corrosion experiments by in situ electron microscopy techniques is not only the achievement of UHV background pressure conditions at the site of the specimen but also the ability to clean the surface of the thin metal substrate specimen before initiation of the corrosive interaction. A miniaturized simple ion gun has been constructed for this purpose. The gun is small enough to be incorporated into an UHV electron microscope specimen chamber with hot stage in such a way as to permit bombardment of the substrate specimen while observing it by transmission electron microscopy TEM. It is shown that the ion beam generated is confined well enough to cause a sputtering removal of substrate material at a rate of approximately 5-10 A/min and to prevent the sputter deposition of contaminating material from the specimen holder.
Heinemann, K.↗
Investigation of interfacial shear strength in SiC/Si3N4 composites
A fiber push-out technique was used to determine fiber/matrix interfacial shear strength (ISS) for silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composites in the as-fabricated condition and after consolidation by hot isostatic pressing (HIPing). In situ video microscopy and acoustic emission detection greatly aided the interpretation of push-out load/displacement curves.
Eldridge, J. I.↗
Investigation of interfacial shear strength in SiC/Si3N4 composites
A fiber push-out technique was used to determine fiber/matrix interfacial shear strength (ISS) for silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composites in the as-fabricated condition and after consolidation by hot isostatic pressing (HIPing). In situ video microscopy and acoustic emission detection greatly aided the interpretation of push-out load/displacement curves.
Eldridge, J. I.↗
Failure mechanisms of 3-D woven SiC/SiC composites under tensile and flexural loading at room and elevated temperatures
Nicalon silicon carbide 3D yarn with silicon carbide matrix composites made through a chemical vapor infiltration (CVI) process were investigated under tensile and flexural loading at 23, 1200 and 1550 C in air. The effectiveness of a chemical vapor deposition (CVD) SiC surface coating was also evaluated in severe oxidizing environment. Acoustic emission sensors and in situ optical microscopy were used at room temperature to monitor the failure mechanisms. It is shown that the level of tensile stress at which nonlinear behavior begins is not drastically reduced at 1200 and 1550 C when composites were protected by a SiC surface coating. Extensive fiber pull-out was observed only in the 1550 C specimen. Similar behaviors were also found in flexural specimens.
Chulya, Abhisak↗
The Structural Properties of Vapor Deposited Water Ice and Astrophysical Implications
Films of vapor deposited water ice at low temperature (T<30 K) show a number of interesting structural changes during a gradual warmup. We would like to talk about the structure of the low temperature high density amorphous form of water ice, the process of crystallization, and some recent work on the morphological changes of water ice films at high temperature. The studies of the high density amorphous form are from in-situ electron microscopy as well as numerical simulations of molecular dynamics and have lead to new insights into the physical distinction between this high density amorphous form and the low density amorphous form. For the process of crystallization, we propose a model that describes the crystallization of water ice from the amorphous phase to cubic ice in terms of the nucleation of small domains in the ice. This model agrees well with the behavior of water ice in our electron microscopy studies and finds that pure water above the glass transition is a strong liquid. In more recent work, we have concentrated on temperatures above the crystallization temperature and we find interesting morphological changes related to the decrease in viscosity of the amorphous component in the cubic crystalline regime. Given enough time, we would like to put these results in an astrophysical context and discuss some observed features of the frost on interstellar grains and the bulk ice in comets.
Jenniskens, P.↗