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Alpha-null defocus: An optimum defocus condition with relevance for focal-series reconstruction

Description: Two optimum defocus conditions are used in high-resolution transmission electron microscopy. Scherzer defocus produces an image of the specimen ''projected potential'' to the resolution of the microscope, and Lichte defocus minimizes dispersion. A third optimum defocus is best for focal-series reconstruction; alpha-null defocus maximizes transfer of high-frequency diffracted beam amplitudes into the microscope image. Beam transfer is confined by incident-beam convergence to a Gaussian ''packet'' of defocus values centered on the alpha-null defocus. For a diffracted beam hkl, with a spatial frequency of u, the envelope for incident beam convergence has null damping effect when defocus is set to -Cs. (wavelength.u)**2. On either side of this alpha-null defocus value, the damping effect of incident-beam convergence reduces diffracted-beam transfer. The position of alpha-null defocus for any spatial frequency depends only on the value of Cs, but defocus-packet width around the alpha-null defocus depends only on the convergence semi-angle. Under NCEM OAM (one-Angstrom microscope) conditions, a [110] diamond image with the correct 0.89A spacing appears when the Si (004) alpha-null defocus is selected. The alpha-null defocus should be included as the (furthest underfocus) limit for all high-resolution focal series reconstruction.
Date: February 14, 2001
Creator: O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Experiences with remote electron microscopy

Description: With the advent of a rapidly proliferating international computer network, it became feasible to consider remote operation of instrumentation normally operated locally. For modern electron microscopes, the growing automation and computer control of many instrumental operations facilitated the task of providing remote operation. In order to provide use of NCEM TEMs by distant users, a project was instituted in 1995 to place a unique instrument, a Kratos EM-1500 operating at 1.5MeV, on-line for remote use. In 1996, the Materials Microcharacterization Collaboratory (MMC) was created as a pilot project within the US Department of Energy's DOE2000 program to establish national collaboratories to provide access via the Internet to unique or expensive DOE research facilities as well as to expertise for remote collaboration, experimentation, production, software development, modeling, and measurement. A major LBNL contribution to the MMC was construction of DeepView, a microscope-independent computer-control system that could be ported to other MMC members to provide a common graphical user-interface (GUI) for control of any MMC instrument over the wide area network.
Date: February 22, 2002
Creator: O'Keefe, Michael A. & Parvin, Bahram
Partner: UNT Libraries Government Documents Department

OLIS: On-Line Image Simulation and structure characterization for the Materials Microcharacterization Collaboratory

Description: On-Line Image Simulation (OLIS) will be made available to remote users from an MMC compute server. OLIS has an interactive GUI to allow users to enter and modify data interactively. OLIS is also integrated with the MMC DeepView control GUI, and OLIS images can thus be displayed on the remote user monitor adjacent to the (live or captured) experimental image, together with a difference image and a goodness-of-fit parameter.
Date: February 13, 1999
Creator: O'Keefe, Michael A. & Taylor, John R.
Partner: UNT Libraries Government Documents Department

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

Defocus step size of the LBNL One Angstrom Microscope

Description: The change in focus of a high-resolution electron microscope is generally assumed to be linear with change in objective lens current. Thus the defocus step size should be constant for a constant step in lens current. Measurements on the LBNL One-Angstrom Microscope show that the step size increases with increasing underfocus (reduced lens current). Differentiation of the best-fit quadratic shows that the defocus step size varies linearly as defocus changes.
Date: July 2, 2002
Creator: O'Keefe, Michael A. & Nelson, E. Chris
Partner: UNT Libraries Government Documents Department

HRTEM at half-Angstrom resolution: From OAM to TEAM

Description: Transmission electron microscopy (TEM) at sub-Angstrom resolution is important for nanotechnology. Identifying atom positions requires appropriate resolution, the ability to separate distinct objects in images. With Cs corrected, the information limit of the TEM controls resolution. The OAM has demonstrated that a resolution of 0.78A is possible. The TEAM (transmission electron achromatic microscope) will be a TEM using hardware correction of Cs with a monochromator to improve its information limit beyond that of the OAM by improvement of the electron-beam energy spread. It is shown that A 300keV HRTEM TEAM does not require a Cc corrector to reach 0.5A as long as beam energy spread and objective-lens current ripple are lowered sufficiently. A lower-voltage TEAM will require stricter limits on objective-lens current ripple to reach the targeted 0.5A resolution. No improvement in HT ripple or noise is required to improve the information limit per se since the monochromator determines the energy spread in the beam. However, improved HT ripple and noise will improve the beam current statistics (number of electrons passing through the monochromator) by placing more of the electrons closer to the center of the energy-spread distribution
Date: February 17, 2003
Creator: O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

One-Angstrom microscope update

Description: The One-Angstrom Microscope project has attained its goal, and is now producing images down to 1 Angstrom resolution. We have demonstrated transmission electron microscopy of defect structures down to a resolution of 1.1 Angstrom, with evidence that 0.89 Angstrom will be possible. This level of resolution will soon be made available to all those NCEM users who have a requirement for sub-Angstrom resolution.
Date: April 4, 1999
Creator: O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Sub-Angstrom resolution with aberration-corrected TEM: Present and future

Description: Resolution is the ability to determine if a feature in an image represents two objects rather than one. Rayleigh's resolution criterion, an accepted standard in optics, was derived as a means for judging when two sources of light (stars) were distinguishable from a single source. In microscopy, resolution is the ability to determine if detail in an image represents distinct (separated) objects. In high-resolution TEM, these objects are atoms. Resolution of |d| is achieved when atoms separated by a (projected) distance |d| can be perceived as separate objects. TEM images are able to depict projected atom columns because they are interference patterns of the directly transmitted electron beam with beams diffracted from the specimen imaged under well-established conditions.
Date: July 1, 2004
Creator: O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Sub-Angstrom Atomic-Resolution Imaging of Heavy Atoms to Light Atoms

Description: Three decades ago John Cowley and his group at ASU achieved high-resolution electron microscope images showing the crystal unit cell contents at better than 4Angstrom resolution. Over the years, this achievement has inspired improvements in resolution that have enabled researchers to pinpoint the positions of heavy atom columns within the cell. More recently, this ability has been extended to light atoms as resolution has improved. Sub-Angstrom resolution has enabled researchers to image the columns of light atoms (carbon, oxygen and nitrogen) that are present in many complex structures. By using sub-Angstrom focal-series reconstruction of the specimen exit surface wave to image columns of cobalt, oxygen, and lithium atoms in a transition metal oxide structure commonly used as positive electrodes in lithium rechargeable batteries, we show that the range of detectable light atoms extends to lithium. HRTEM at sub-Angstrom resolution will provide the essential role of experimental verification for the emergent nanotech revolution. Our results foreshadow those to be expected from next-generation TEMs with Cs-corrected lenses and monochromated electron beams.
Date: May 23, 2003
Creator: O'Keefe, Michael A. & Shao-Horn, Yang
Partner: UNT Libraries Government Documents Department

Estimation of the electron beam energy spread for TEM information limit

Description: Sub-Angstrom TEM of materials requires focal-series reconstruction (FSR) or electron holography to retrieve the electron wave at the specimen exit-surface to very high resolution. As a consequence, we need to measure the microscope information limit. With a sub-Angstrom information limit, the one-Angstrom microscope (OAM) project at the NCEM has achieved sub-Angstrom resolution by FSR. We present a new method of estimating the information limit of the microscope, based on energy-spread measurements with an image filter.
Date: February 20, 2002
Creator: O'Keefe, Michael A.; Tiemeijer, Peter C. & Sidorov, Maxim V.
Partner: UNT Libraries Government Documents Department

Dislocation core in GaN

Description: Light emitting diodes and blue laser diodes grown on GaN have been demonstrated despite six orders of magnitude higher dislocation density than that for III-V arsenide and phosphide diodes. Understanding and determination of dislocation cores in GaN is crucial since both theoretical and experimental work are somewhat contradictory. Transmission Electron Microscopy (TEM) has been applied to study the layers grown by hydride vapor-phase epitaxy (HVPE) and molecular beam epitaxy (MBE) (under Ga rich conditions) in plan-view and cross-section samples. This study suggests that despite the fact that voids are formed along the dislocation line in HVPE material, the dislocations have closed cores. Similar results of closed core are obtained for the screw dislocation in the MBE material, confirming earlier studies.
Date: February 20, 2002
Creator: Liliental-Weber, Zuzanna; Jasinski, Jacek B.; Washburn, Jack & O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Measurement of the energy-spread contribution to information transfer limits in HR-TEM

Description: Sub-Angstrom TEM of materials at intermediate voltages requires a sub-Angstrom information limit for the microscope. With a Scherzer resolution of 1.7 Angstrom, but a sub-Angstrom information limit, the one-Angstrom microscope (OAM) project at the NCEM is able to generate resolution below 0.8 Angstrom. Microscope information limit comes from damping of transfer by the temporal coherence. A major term contributing to temporal coherence is energy spread in the electron beam. We derive a new expression for the energy spread, and show how it can be measured from the result that is obtained using a standard electron spectrometer.
Date: February 18, 2002
Creator: O'Keefe, Michael A.; Tiemeijer, Peter C. & Sidorov, Maxim V.
Partner: UNT Libraries Government Documents Department

Sub-Angstrom transmission electron microscopy at 300keV

Description: We have demonstrated sub-Angstrom TEM to a resolution of 0.78 Angstrom with the one-Angstrom microscope (OAM) project at the National Center for Electron Microscopy. The OAM combines a modified CM300FEG-UT with computer software able to generate sub-Angstrom images from experimental image series. We achieved sub-Angstrom resolution with the OAM by paying close attention to detail. We placed the TEM in a favorable environment. We reduced its three-fold astigmatism A2 from 2.46mm to 300 Angstrom (corresponding to transfer of 0.68 Angstrom spacings at a pi/4 phase limit). We improved its information limit by minimizing high-voltage and lens current ripple. Energy spread of 0.93eV FWHH gave a focus spread of 20 Angstrom and an information limit of 0.78 Angstrom, allowing successful resolution of the 0.89 Angstrom (400) atom spacings in [110] diamond. As a further test, we reduced the electron gun extraction voltage to 3kV to improve our information limit to 0.75 Angstrom, and then imaged 0 .7 Angstrom (444) atom spacings in [112] silicon as distinct pairs of 'white atoms' near an alpha-null defocus of -3783 Angstrom.
Date: February 14, 2001
Creator: O'Keefe, Michael A.; Nelson, E. Christian; Turner, John H. & Thust, Andreas
Partner: UNT Libraries Government Documents Department

Atomic resolution 3D electron diffraction microscopy

Description: Electron lens aberration is the major barrier limiting the resolution of electron microscopy. Here we describe a novel form of electron microscopy to overcome electron lens aberration. By combining coherent electron diffraction with the oversampling phasing method, we show that the 3D structure of a 2 x 2 x 2 unit cell nano-crystal (framework of LTA [Al12Si12O48]8) can be ab initio determined at the resolution of 1 Angstrom from a series of simulated noisy diffraction pattern projections with rotation angles ranging from -70 degrees to +70 degrees in 5 degrees increments along a single rotation axis. This form of microscopy (which we call 3D electron diffraction microscopy) does not require any reference waves, and can image the 3D structure of nanocrystals, as well as non-crystalline biological and materials science samples, with the resolution limited only by the quality of sample diffraction.
Date: March 1, 2002
Creator: Miao, Jianwei; Ohsuna, Tetsu; Terasaki, Osamu & O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

HRTEM image simulations for gate oxide metrology

Description: High resolution transmission electron microscopy (HRTEM) has found extensive use in the semiconductor industry for performing device metrology and characterization. However, shrinking device dimensions (gate oxides are rapidly approaching 10{angstrom}) present challenges to the use of HRTEM for many applications, including gate oxide metrology. In this study, we performed HRTEM image simulations of a MOSFET device to examine the accuracy of HRTEM in measuring gate oxide thickness. Length measurements extracted from simulated images were compared to actual dimensions in the model structure to assess TEM accuracy. The effects of specimen tilt, specimen thickness, objective lens defocus and coefficient of spherical aberration (C{sub s}) on measurement accuracy were explored for nominal 10{angstrom} and 16{angstrom} gate oxide thicknesses. The gate oxide was modeled as an amorphous silicon oxide situated between a gate electrode and substrate, both modeled as single crystal Si(100). Image simulations of the sandwich structure were performed in cross-section (with Si[110] parallel to beam direction) using the multislice approximation for a 200 kV microscope with C{sub s}=0.5mm. Amorphous slices were added to the top and bottom of the specimen to simulate the amorphization that occurs during typical specimen preparation. The actual gate oxide thickness, T, is defined as the distance between the bounding Si atoms in the model structure. The gate oxide thickness was also measured directly in pixels from the simulated image. We use a statistical routine to calculate the standard deviation in pixel intensity for each horizontal row (or y-coordinate) in the simulated image. Local minima in the standard deviation, which correspond to low-intensity regions between Si[110] dumbbells, were used to calibrate the image length scale. The measured gate oxide thickness was then compared to the actual (model) thickness to assess accuracy for a variety of microscope and specimen conditions. Results reveal no consistent trends in measurement accuracy ...
Date: February 10, 2000
Creator: Taylor, Seth; Mardinly, John; O'Keefe, Michael A. & Gronsky, R.
Partner: UNT Libraries Government Documents Department

Focal-series reconstruction of nanoparticle exit-surface electron wave

Description: We have used the One-Angstrom Microscope (OAM) to image and apply focal-series reconstruction (FSR) of the exit-surface wave (ESW) to a 70Angstrom particle of gold supported on amorphous carbon. The phase of the complex ESW shows the positions of the atom columns in the specimen as white dots, and its diffractogram shows it contains information to 1.23Angstrom. The result demonstrates that through-focal reconstruction of the ESW does not need large crystal expanses to work properly. Although [110] Au structures may not need sub-Angstrom resolution to show all the useful structural details of the particle in this orientation, it is clear that focal reconstruction of the ESW can improve original data that is much more difficult to interpret directly. We expect this technique to prove even more useful when applied to nanoparticles containing finer spacings than the 2.35Angstrom separation of the 111 planes in the present gold nano-particle.
Date: February 24, 2003
Creator: O'Keefe, Michael A.; Nelson, E.Chris & Allard, Lawrence F.
Partner: UNT Libraries Government Documents Department

Atomic-Resolution 3D Electron Microscopy with Dynamic Diffraction

Description: Achievement of atomic-resolution electron-beam tomography will allow determination of the three-dimensional structure of nanoparticles (and other suitable specimens) at atomic resolution. Three-dimensional reconstructions will yield ''section'' images that resolve atoms overlapped in normal electron microscope images (projections), resolving lighter atoms such as oxygen in the presence of heavier atoms, and atoms that lie on non-lattice sites such as those in non-periodic defect structures. Lower-resolution electron microscope tomography has been used to produce reconstructed 3D images of nanoparticles [1] but extension to atomic resolution is considered not to be straightforward. Accurate three-dimensional reconstruction from two-dimensional projections generally requires that intensity in the series of 2-D images be a monotonic function of the specimen structure (often specimen density, but in our case atomic potential). This condition is not satisfied in electron microscopy when specimens with strong periodicity are tilted close to zone-axis orientation and produce ''anomalous'' image contrast because of strong dynamic diffraction components. Atomic-resolution reconstructions from tilt series containing zone-axis images (with their contrast enhanced by strong dynamical scattering) can be distorted when the stronger zone-axis images overwhelm images obtained in other ''random'' orientations in which atoms do not line up in neat columns. The first demonstrations of 3-D reconstruction to atomic resolution used five zone-axis images from test specimens of staurolite consisting of a mix of light and heavy atoms [2,3]. Initial resolution was to the 1.6{angstrom} Scherzer limit of a JEOL-ARM1000. Later experiments used focal-series reconstruction from 5 to 10 images to produce staurolite images from the ARM1000 with resolution extended beyond the Scherzer limit to 1.38{angstrom} [4,5]. To obtain a representation of the three-dimensional structure, images were obtained in zone-axis projections <100>, <010>, <001>, <101>, <310>, and combined to produce a three-dimensional map of Coulomb potential. Images of specimen sections are much more easily interpreted than projection images ...
Date: February 15, 2005
Creator: O'Keefe, Michael A.; Downing, Kenneth H.; Wenk, Hans-Rudolf & Meisheng, Hu
Partner: UNT Libraries Government Documents Department

Pyramidal Defects in GaN:Mg Grown with Ga Polarity

Description: Transmission electron microscopy (TEM) studies show formation of different types of Mg-rich defects in GaN. Types of defects strongly depend on crystal growth polarity. For bulk crystals grown with N-polarity, the planar defects are distributed at equal distances (20 unit cells of GaN). For growth with Ga-polarity (for both bulk and MOCVD grown crystals) a different type of defects have been found. These defects are three-dimensional Mg-rich hexagonal pyramids (or trapezoids) with their base on the (0001) plane and six walls formed on 1123 planes. The defects appear in [1120] and [1100] cross-section TEM micrographs as triangular and trapezoidal with sides inclined at 43 and 47 degrees to the base depending on the above observation directions, respectively. The dimension of these pyramids varies depending on growth method (50-1000 Angstrom), but the angle between the base and their sides remain the same. The direction from the tip of the pyramid to its base (and from the shorter to the longer base for trapezoidal defects) is along the Ga to N matrix bond direction. Analysis of the reconstructed exit wave phase image from the pyramid side indicates a shift of Ga atomic column positions from the matrix to the N position within the pyramid. In this way a 0.6{+-}0.2 Angstrom displacement can be measured on the pyramid side between Ga positions in the matrix and within the pyramid.
Date: February 15, 2005
Creator: Liliental-Weber, Zuzanna; Tomaszewicz, Tomasz; Zakharov, Dmitri & O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Resolution Quality and Atom Positions in Sub-Angstrom Electron Microscopy

Description: Ability to determine whether an image peak represents one single atom or several depends on resolution of the HR-(S)TEM. Rayleigh's resolution criterion, an accepted standard in optics, was derived as a means for judging when two image intensity peaks from two sources of light (stars) are distinguishable from a single source. Atom spacings closer than the Rayleigh limit have been resolved in HR-TEM, suggesting that it may be useful to consider other limits, such as the Sparrow resolution criterion. From the viewpoint of the materials scientist, it is important to be able to use the image to determine whether an image feature represents one or more atoms (resolution), and where the atoms (or atom columns) are positioned relative to one another (resolution quality). When atoms and the corresponding image peaks are separated by more than the Rayleigh limit of the HR-(S)TEM, it is possible to adjust imaging parameters so that relative peak positions in the image correspond to relative atom positions in the specimen. When atoms are closer than the Rayleigh limit, we must find the relationship of the peak position to the atom position by peak fitting or, if we have a suitable model, by image simulation. Our Rayleigh-Sparrow parameter QRS reveals the ''resolution quality'' of a microscope image. QRS values greater than 1 indicate a clearly resolved twin peak, while values between 1 and 0 mean a lower-quality resolution and an image with peaks displaced from the relative atom positions. The depth of the twin-peak minimum can be used to determine the value of QRS and the true separation of the atom peaks that sum to produce the twin peak in the image. The Rayleigh-Sparrow parameter can be used to refine relative atom positions in defect images where atoms are closer than the Rayleigh limit of the HR-(S)TEM, ...
Date: February 15, 2005
Creator: O'Keefe, Michael A.; Allard, Lawrence F. & Blom, Douglas A.
Partner: UNT Libraries Government Documents Department

HRTEM image simulations for the study of ultra-thin gate oxides

Description: We have performed high resolution transmission electron microscope (HRTEM) image simulations to qualitatively assess the visibility of various structural defects in ultra-thin gate oxides of MOSFET devices, and to quantitatively examine the accuracy of HRTEM in performing gate oxide metrology. Structural models contained crystalline defects embedded in an amorphous 16 {angstrom}-thick gate oxide. Simulated images were calculated for structures viewed in cross-section. Defect visibility was assessed as a function of specimen thickness and defect morphology, composition, size and orientation. Defect morphologies included asperities lying on the substrate surface, as well as ''bridging'' defects connecting the substrate to the gate electrode. Measurements of gate oxide thickness extracted from simulated images were compared to actual dimensions in the model structure to assess TEM accuracy for metrology. The effects of specimen tilt, specimen thickness, objective lens defocus and coefficient of spherical aberration (C{sub s}) on measurement accuracy were explored for nominal 10{angstrom} gate oxide thickness. Results from this work suggest that accurate metrology of ultra-thin gate oxides (i.e. limited to several per cent error) is feasible on a consistent basis only by using a C{sub s}-corrected microscope. However, fundamental limitations remain for characterizing defects in gate oxides using HRTEM, even with the new generation of C{sub s}-corrected microscopes.
Date: July 17, 2001
Creator: Taylor, Seth T.; Mardinly, John & O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Screw dislocations in GaN

Description: GaN has received much attention over the past few years because of several new applications, including light emitting diodes, blue laser diodes and high-power microwave transistors. One of the biggest problems is a high density of structural defects, mostly dislocations, due to a lack of a suitable lattice-matched substrate since bulk GaN is difficult to grow in large sizes. Transmission Electron Microscopy (TEM) has been applied to study defects in plan-view and cross-sections on samples prepared by conventional techniques such as mechanical thinning and precision ion milling. The density of dislocations close to the sample surface of a 1 mm-thick HVPE sample was in the range of 3x109 cm-2. All three types of dislocations were present in these samples, and almost 50 percent were screw dislocations. Our studies suggest that the core structure of screw dislocations in the same material might differ when the material is grown by different methods.
Date: February 15, 2002
Creator: Liliental-Weber, Zuzanna; Jasinski, Jacek B.; Washburn, Jack & O'Keefe, Michael A.
Partner: UNT Libraries Government Documents Department

Reaching sub-Angstrom resolution with a mid-voltage TEM

Description: Phase-contrast imaging in the high-resolution electron microscope produces images with peaks at atom positions by extracting the spatial distribution of the relative phase from the electron wave. Usually, the electron wave is imaged by direct interference of diffracted beams at optimum focus. Instead, the One-Angstrom Microscope uses focal-series reconstruction software to derive the relative electron phase from a series of images taken over a range of focus, with peaks that correspond to the atom positions at a resolution that extends to the microscope information limit. Tests using a silicon specimen tilted into [112] orientation show that the O Angstrom M has achieved a world-record resolution of 0.78 Angstrom.
Date: April 12, 2004
Creator: O'Keefe, Michael A.; Hetherington, Crispin J.D. & Nelson, E. Chris
Partner: UNT Libraries Government Documents Department