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The optimum Cs condition for high-resolution transmission electron microscopy

Description: With the advent of electron-optical systems able to generate negative spherical aberration (usually called ''Cs correctors''), it has now become feasible to zero-out objective lens Cs in the high-resolution transmission electron microscope. However, I show that - instead of tuning out spherical aberration completely - there is an optimum value for the residual Cs that maximizes information transfer to the best possible resolution and depends only on the information limit of the microscope.
Date: February 14, 2000
Creator: O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Large melting point hysteresis of Ge nanocrystals embedded inSiO2

Description: The melting behavior of Ge nanocrystals embedded within SiO{sub 2} is evaluated using in situ transmission electron microscopy. The observed melting point hysteresis is large ({+-} 17%) and nearly symmetric about the bulk melting point. This hysteresis is modeled successfully using classical nucleation theory without the need to invoke epitaxy.
Date: May 4, 2006
Creator: Xu, Q.; Sharp, I.D.; Yuan, C.W.; Yi, D.O.; Liao, C.Y.; Glaeser,A.M. et al.
Partner: UNT Libraries Government Documents Department

Study of dislocations in copper by weak beam, stereo, and in situ straining TEM

Description: Conventional transmission electron microscopy (TEM) has been an invaluable tool for verifjhg and developing dislocation theories since the first direct observations of dislocations were made using a TEM in the 1950s. Several useful techniques and technological advancements have been made since, helping fbrther the advancement of dislocation knowledge. The present paper concerns two studies of dislocations in copper made by coupling several of these techniques, specifically weak beam, in situ straining, and stereo TEM. Stereo-TEM coupled with in situ straining TEM was used for tracking 3D dislocation motion and interactions in low dislocation density copper foils. A mechanism by which dislocations in a pileup bypass a dislocation node is observed and discussed. Weak beam TEM is used in conjunction with stereo-TEM to analyze the dislocation content of a dense dislocation wall (DDW).
Date: January 1, 2002
Creator: McCabe, R. J. (Rodney J.); Misra, A. (Amit) & Mitchell, T. E. (Terence E.)
Partner: UNT Libraries Government Documents Department

Transmission Electron Microscopy Characterization of Nanocrystalline Copper

Description: The microstructure and grain boundary structure of nanocrystalline Cu powders and a compact prepared by the inert-gas condensation technique have been characterized by transmission electron microscopy. The as-prepared particles are round in shape and have no distinct surface facets. Annealing twins (coherent {Sigma}3 boundaries) have been observed in the as-prepared Cu particles as well as in the compact. Pores are commonly found at grain boundaries, triple grain junctions and some in the interior of grains in the compact. In addition to twin boundaries, a number of special grain boundaries have been observed. These special grain boundaries have low-index interface planes, and sometimes have misorientation angles close to coincidence site lattice (CSL) orientations.
Date: November 1, 1999
Creator: Kung, H.; Sanders, P.G. & Weertman, J.R.
Partner: UNT Libraries Government Documents Department

In-situ nanoindentation specimen holder for a high-voltage transmission electron microscope

Description: This report describes the design, construction, and testing of a nanoindentation specimen holder used for dynamic observation of subsurface microstructure evolution under an indenter tip, while viewing in cross-section in a high-voltage transmission electron microscope (TEM). It also discusses the initial experimental results from in-situ indentation of Si samples in the TEM to demonstrate the capability of this new nanoindentation specimen holder, which uses three-axis position control of a diamond indenter in combination with micromachined specimens. Additionally, the sample design techniques developed for these procedures may eliminate the need for TEM specimen preparation in future ex-situ nanoindentation experiments and for sample preparation for characterizing these experiments in the electron microscope.
Date: September 17, 1998
Creator: Dahmen; U & Wall, M A
Partner: UNT Libraries Government Documents Department

Microstructural Studies of Dental Amalgams Using Analytical Transmission Electron Microscopy

Description: Dental amalgams have been used for centuries as major restorative materials for decaying teeth. Amalgams are prepared by mixing alloy particles which contain Ag, Sn, and Cu as the major constituent elements with liquid Hg. The study of microstructure is essential in understanding the setting reactions and improving the properties of amalgams. Until the work reported in this dissertation, optical microscopy (OM), scanning electron microscopy (SEM), and x-ray diffractometry (XRD) were used commonly to analyze amalgam microstructures. No previous systematic transmission electron microscopy (TEM) study has been performed due to sample preparation difficulties and composite structure of dental amalgams. The goal of this research was to carry out detailed microstructural and compositional studies of dental amalgams. This was accomplished using the enhanced spatial resolution of the TEM and its associated microanalytical techniques, namely, scanning transmission electron microscopy (STEM), x-ray energy dispersive spectroscopy (XEDS) and micro-microdiffraction (μμD). A new method was developed for thinning amalgam samples to electron transparency using the "wedge technique." Velvalloy, a low-Cu amalgam, and Tytin, a high-Cu amalgam, were the two amalgams characterized. Velvalloy is composed of a Ag₂Hg₃ (γ₁)/HgSn₇₋₉ (γ₂) matrix surrounding unreacted Ag₃Sn (γ) particles. In addition, hitherto uncharacterized reaction layers between Ag₃Sn(γ)/Ag₂Hg₃ (γ₂) and Ag₂Hg₃ (γ₁)/HgSn₇₋₉ (γ₂) were observed and analyzed. An Ag-Hg-Sn (β₁) phase was clearly identified for the first time. In Tytin, the matrix consists of Ag₂Hg₃ (γ₁) grains. Fine precipitates of Cu₆Sn₅ (η') are embedded inside the γ₁ and at the grain boundaries. These precipitates are responsible for the improved creep resistance of Tytin compared to Velvalloy. The additional Cu has completely eliminated the γ₂ phase which is the weakest component of amalgams. Ag-Hg-Sn (β₁) and large grains of Cu₆Sn₅ (η') are found adjacent to the unreacted alloy particles. Tytin alloy particles contain Cu₃Sn (ε) precipitates in a matrix of Ag₃Sn ...
Date: May 1997
Creator: Hooghan, Tejpal Kaur
Partner: UNT Libraries

Atomic Structure and Properties of Extended Defects in Silicon

Description: The Z-contrast technique represents a new approach to high-resolution electron microscopy allowing for the first time incoherent imaging of materials on the atomic scale. The key advantages of the technique, an intrinsically higher resolution limit and directly interpretable, compositionally sensitive imaging, allow a new level of insight into the atomic configurations of extended defects in silicon. This experimental technique has been combined with theoretical calculations (a combination of first principles, tight binding, and classical methods) to extend this level of insight by obtaining the energetic and electronic structure of the defects.
Date: October 15, 1998
Creator: Buczko, R.; Chisholm, M.F.; Kaplan, T.; Maiti, A.; Mostoller, M.; Pantelides, S.T. et al.
Partner: UNT Libraries Government Documents Department

Analyses of Particulate Contaminants in Semiconductor Processing Fluids

Description: Particle contamination control is a critical issue for the semiconductor industry. In the near future, this industry will be concerned with the chemical identities of contaminant particles as small as 0.01 pm in size. Therefore, analytical techniques with both high chemical sensitivity and spatial resolution are required. Transmission electron microscopy (TEM) provides excellent spatial resolution and yields structural and compositional information. It is rarely used, however, due to the difficulty of sample preparation. The goals of this research are to promote the use of TEM as an ultrafine particle analysis tool by developing new sample preparation methods, and to exploit the new TEM techniques for analysis of particles in semiconductor processing fluids. A TEM methodology for the analysis of particulate contaminants in fluids with an elemental detectability limit as low as 0.1 part per trillion (ppt), and a particle concentration detectability limit as low as 1 particle/ml for particles greater than 0.2 pm was developed and successfully applied to the analysis of particles in HF, H202, de-ionized (DI) water, and on the surface of an electronic device. HF samples from three manufacturers were examined. For HF (B), the maximum particle concentration was 8.3 x 103 particles/ml. Both a viscous material and lath-shaped particles were observed. The Sb concentration was less than 0.6 part per billion (ppb). HF (C) was the cleanest. CaF2 and TiO2 particles were identified in HF (D). For H2 02, iron and tin oxides and hydroxides were identified. The maximum particle concentration was 990 particles/ml. The Sn and Fe concentrations were less than 0.3 ppb. Spherical and dendritic particles were observed. For DI water, spherical and dendritic particles (<2 particles/ml), and particles containing Fe or Si with concentrations less than 0.1 ppt were observed. Contaminants on an electronic device surface were also analyzed. Clusters of small particles ...
Date: August 1998
Creator: Xu, Daxue
Partner: UNT Libraries

Development of a nanoindenter for in-situ transmission electron microscopy

Description: In-situ transmission electron microscopy is an established experimental technique that permits direct observation of the dynamics and mechanisms of dislocation motion and deformation behavior. In this paper, we detail the development of a novel specimen goniometer that allows real time observations of the mechanical response of materials to indentation loads. The technology of the scanning tunneling microscope is adopted to allow nanometer scale positioning of a sharp, conductive diamond tip onto the edge of an electron transparent sample. This allows application of loads to nanometer-scale material volumes couple with simultaneous imaging of the material response. The emphasis in this paper is experimental and descriptive, with particular attention given to sample geometry and other technical requirements. Examples of the deformation of aluminum and titanium carbide as well as the fracture of silicon will be presented.
Date: January 30, 2001
Creator: Stach, Eric A.; Freeman, Tony; Minor, Andrew M.; Owen, Doug K.; Cumings, John; Wall, Mark A. et al.
Partner: UNT Libraries Government Documents Department

In-situ TEM - a tool for quantitative observations of deformation behavior in thin films and nano-structured materials

Description: This paper highlights future developments in the field of in-situ transmission electron microscopy, as applied specifically to the issues of deformation in thin films and nanostructured materials. Emphasis is place on the forthcoming technical advances that will aid in extraction of improved quantitative experimental data using this technique.
Date: September 4, 2001
Creator: Stach, E.A.
Partner: UNT Libraries Government Documents Department

Nitrogen effects on crystallization kinetics of amorphous TiOxNy thin films

Description: The crystallization behavior of amorphous TiOxNy (x&gt;&gt;y) thin films was investigated by in-situ transmission electron microscopy. The Johnson-Mehl-Avrami-Kozolog (JMAK) theory is used to determine the Avrami exponent, activation energy, and the phase velocity pre-exponent. Addition of nitrogen inhibits diffusion, increasing the nucleation temperature, while decreasing the growth activation energy. Kinetic variables extracted from individual crystallites are compared to JMAK analysis of the fraction transformed and a change of 6 percent in the activation energy gives agreement between the methods. From diffraction patterns and index of refraction the crystallized phase was found to be predominantly anatase.
Date: March 30, 2001
Creator: Hukari, Kyle; Dannenberg, Rand & Stach, E.A.
Partner: UNT Libraries Government Documents Department

Specimen charging on thin films with one conducting layer:Discussion of physical principles

Description: While the most familiar consequences of specimen charging in transmission electron microscopy can be eliminated by evaporating a thin conducting film (such as a carbon film) onto an insulating specimen, or by preparing samples directly on such a conducting film to begin with, a more subtle charging effect still remains. We argue here that specimen charging is in this case likely to produce a dipole sheet rather than a layer of positive charge at the surface of the specimen. A simple model of the factors that control the kinetics of specimen charging, and its neutralization, is discussed as a guide for experiments that attempt to minimize the amount of specimen charging. Believable estimates of the electrostatic forces and the electron optical disturbances that are likely to occur suggest that specimen bending and warping may have the biggest impact on degrading the image quality at high resolution. Electron optical effects are likely to be negligible except in the case of a specimen that is tilted to high angle. A model is proposed to explain how both the mechanical and electron-optical effects of forming a dipole layer would have much greater impact on the image resolution in a direction perpendicular to the tilt axis, a well-known effect in electron microscopy of two-dimensional crystals.
Date: April 15, 2003
Creator: Glaeser, Robert M. & Downing, Kenneth H.
Partner: UNT Libraries Government Documents Department

New mechanism for dislocation blocking in strained layer epitaxial growth

Description: Dislocation interactions play a critical role in plasticity and heteroepitaxial strain relaxation. We use real time transmission electron microscopy observations of the interaction between threading and misfit dislocations in SiGe heterostructures to investigate interactions quantitatively. In addition to the expected long range blocking of threading segments, we observe a new short range mechanism which is significantly more effective. Simulations show that this reactive blocking occurs when two dislocations with the same Burgers vector reconnect.
Date: September 14, 1999
Creator: Stach, E.A.; Schwarz, K.W.; Hull, R.; Ross, F.M. & Tromp, R.M.
Partner: UNT Libraries Government Documents Department

Structural, Magnetic and Electronic Properties of (110)-OrientedEpitaxial Thin Films of Bilayer Manganite La1.2Sr1.8Mn2O7

Description: We have synthesized (110)-oriented epitaxial thin films of the bilayer (n=2) manganite, La{sub 1.2}Sr{sub 1.8}Mn{sub 2}O{sub 7}, with the metallic/ferromagnetic a-b planes lying perpendicular to the substrate surface and the c-axis aligned in the plane of the film. X-ray diffraction and transmission electron microscopy confirm the alignment of the a-b planes along the [1{bar 1}0] substrate direction. The films consist primarily of the n=2 phase with a minor component of the n=1 (La,Sr){sub 2}MnO{sub 4} and n={infinity} (La,Sr)MnO{sub 3} phases. A resistivity maximum coincides with a ferromagnet/paramagnet transition at a reduced T{sub c}{approx}90K (vs. 120K for bulk), indicative of the effects of epitaxial strain. The films display similar anisotropic properties to their bulk counterpart with the magnetically easy direction confined to the a-b planes and 20-200 times lower resistivity for current flowing along the a-b planes compared to the c-axis.
Date: May 9, 2005
Creator: Takamura, Yayoi; Grepstad, Jostein K.; Chopdekar, Rajesh V.; Suzuki, Yuri; Marshall, Ann F.; Zheng, Hong et al.
Partner: UNT Libraries Government Documents Department

Al2O3 Scale Development on Iron Aluminides

Description: The structure and phase of the Al{sub 2}O{sub 3} scale that forms on an Fe{sub 3}Al-based alloy (Fe-28Al-5Cr) (at %) was investigated by transmission electron microscopy (TEM) and photoluminescence spectroscopy (PL). Oxidation was performed at 900 C and 1000 C for up to 190 min. TEM revealed that single-layer scales were formed after short oxidation times. Electron diffraction was used to show that the scales are composed of nanoscale crystallites of the {theta}, {gamma}, and {alpha} phases of alumina. Band-like structure was observed extending along three 120{sup o}-separated directions within the surface plane. Textured {theta} and {gamma} grains were the main components of the bands, while mixed {alpha} and transient phases were found between the bands. Extended oxidation produced a double-layered scale structure, with a continuous {alpha} layer at the scale/alloy interface, and a {gamma}/{theta} layer at the gas surface. The mechanism for the formation of Al{sub 2}O{sub 3} scales on iron aluminide alloys is discussed and compared to that for nickel aluminide alloys.
Date: November 10, 2005
Creator: Zhang, Xiao-Feng; Thaidigsmann, Katja; Ager, Joel & Hou, Peggy Y.
Partner: UNT Libraries Government Documents Department

Examination of the local structure in composite and lowdimensional semiconductor by X-ray Absorption Spectroscopy

Description: X-ray absorption methods have been successfully used to obtain quantitative information about local atomic composition of two different materials. X-ray Absorption Near Edge Structure analysis and X-Ray Photoelectron Spectroscopy allowed us to determine seven chemical compounds and their concentrations in c-BN composite. Use of Extended X-ray Absorption Fine Structure in combination with Transmission Electron Microscopy enabled us to determine the composition and size of buried Ge quantum dots. It was found that the quantum dots consisted out of pure Ge core covered by 1-2 monolayers of a layer rich in Si.
Date: September 25, 2006
Creator: Lawniczak-Jablonska, K.; Demchenko, I.N.; Piskorska, E.; Wolska,A.; Talik, E.; Zakharov, D.N. et al.
Partner: UNT Libraries Government Documents Department

Transmission Electron Microscopy Study of InN Nanorods

Description: InN nanorods were grown on a, c-, and r-plane of sapphire and also on Si (111) and GaN (0001) by non-catalytic, template-free hydride metal-organic vapor phase epitaxy and studied by transmission electron microscopy, electron energy loss (EELS) and photoluminescence (PL) at room temperature. These nanocrystals have different shapes and different faceting depending on the substrate used and their crystallographic orientation. EELS measurements have confirmed the high purity of these crystals. The observed PL peak was in the range of 0.9-0.95 eV. The strongest PL intensity was observed for the nanocrystals with the larger diameters.
Date: July 13, 2006
Creator: Liliental-Weber, Z.; Li, X.; Kryliouk, Olga; Park, H.J.; Mangum,J. & Anderson, T.
Partner: UNT Libraries Government Documents Department

InN Nanorods and Epi-layers: Similarities and Differences

Description: Transmission electron microscopy was applied to study InN nanorods grown on the a-, c-and r-plane of Al{sub 2}O{sub 3}, and (111) Si substrates by non-catalytic, template-free hydride metal-organic vapor phase epitaxy (H-MOVPE). Single crystal nanorod growth was obtained on all substrates. However, the shape of the nanorods varied depending on the substrate used. For example, nanorods grown on r-plane sapphire and (111) Si have sharp tips. In contrast, growth on a- and c- planes of Al{sub 2}O{sub 3} results in flat tips with clear facets on their sides. The structural quality of these nanorods and their growth polarity are compared to crystalline quality, surface roughness, defects and growth polarity of InN layers grown by MBE on the same planes of Al{sub 2}O{sub 3}.
Date: March 30, 2007
Creator: Liliental-Weber, Z.; Kryliouk, O.; Park, H.J.; Mangum, J.; Anderson, T. & Schaff, W.
Partner: UNT Libraries Government Documents Department

Three-Dimensional Aberration-Corrected Scanning Transmission Electron Microscopy for Biology

Description: Recent instrumental developments have enabled greatly improved resolution of scanning transmission electron microscopes (STEM) through aberration correction. An additional and previously unanticipated advantage of aberration correction is the greatly improved depth sensitivity that has led to the reconstruction of a three-dimensional (3D) image from a focal series. In this chapter the potential of aberration-corrected 3D STEM to provide major improvements in the imaging capabilities for biological samples will be discussed. This chapter contains a brief overview ofthe various high-resolution 3D imaging techniques, a historical perspective of the development of STEM, first estimates of the dose-limited axial and lateral resolution on biological samples and initial experiments on stained thin sections.
Date: January 1, 2007
Creator: De Jonge, Niels; Sougrat, Rachid; Pennycook, Stephen J; Peckys, Diana B & Lupini, Andrew R
Partner: UNT Libraries Government Documents Department

Sorption Behavior and Morphology of Plutonium in the Presence of Goethite at 25 and 80C

Description: In this study, we examined the sorption behavior of Pu at elevated temperatures in the presence of one relevant mineral, goethite ({alpha}-FeOOH), over a range of concentrations that span solubility-controlled to adsorption-controlled concentrations. We focused on the sorptive behavior of two common forms of Pu: aqueous Pu(IV) and intrinsic Pu(IV) nano-colloids at 25 and 80 C in a dilute pH 8 NaCl/NaHCO{sub 3} solution. The morphology of Pu sorbed to goethite was characterized using transmission electron microscopy (TEM). We examined the relative stability of PuO{sub 2} precipitates, PuO{sub 2} nano-colloids, Pu{sub 4}O{sub 7} surface precipitates, and monomeric sorbed Pu as a function of temperature and over a time scale of months.
Date: June 11, 2012
Creator: Zavarin, M.; Zhao, P.; Dai, Z.; Carroll, S. A. & Kersting, A. B.
Partner: UNT Libraries Government Documents Department

Dynamic response of single crystalline copper subjected to quasi-isentropic laser and gas-gun driven loading

Description: Single crystalline copper was subjected to quasi-isentropic compression via gas-gun and laser loading at pressures between 18 GPa and 59 GPa. The deformation substructure was analyzed via transmission electron microscopy (TEM). Twins and laths were evident at the highest pressures, and stacking faults and dislocation cells in the intermediate and lowest pressures, respectively. The Preston-Tonks-Wallace (PTW) constitutive description was used to model the slip-twinning process in both cases.
Date: May 22, 2006
Creator: Meyers, M; Jarmakani, H; McNaney, J; Schneider, M; Nguyen, J & Kad, B
Partner: UNT Libraries Government Documents Department


Description: A transmission electron microscopy study of quasi-isentropic high-pressure loading (peak pressures between 18 GPa and 52 GPa) of polycrystalline and monocrystalline copper was carried out. Deformation mechanisms and defect substructures at different pressures were analyzed. Current evidence suggests a deformation substructure consisting of twinning at the higher pressures and heavily dislocated laths and dislocation cells at the intermediate and lower pressures, respectively. Evidence of stacking faults at the intermediate pressures was also found. Dislocation cell sizes decreased with increasing pressure and increased with distance away from the surface of impact.
Date: September 29, 2005
Creator: Jarmakani, H; McNaney, J M; Schneider, M S; Orlikowski, D; Nguyen, J H; Kad, B et al.
Partner: UNT Libraries Government Documents Department

Final Report LDRD 04-ERD-021

Description: In this project, we performed experiments and simulations to establish constitutive models for plastic behavior and to determine the deformation mechanism of nanocrystalline materials at different grain sizes (&lt;100 nm) and high strain rates (&gt;10{sup 6}/s). The experiments used both laser-induced shocks and isentropic compression to investigate, for the first time, the high-strain-rate deformation of nanocrystalline Ni. Samples were characterized using transmission electron microscopy, nanoindentation, profilometry, and x-ray diffraction before and after loading. We validated constitutive models using both atomistic molecular dynamics and continuum simulations performed at the boundary of their current computational possibilities to match experimental scales.
Date: February 23, 2007
Creator: Bringa, E
Partner: UNT Libraries Government Documents Department