Edward R. White

Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution

Dislocations and their interactions strongly influence many material properties, ranging from the strength of metals and alloys to the efficiency of light-emitting diodes and laser diodes. Several experimental methods can be used to visualize dislocations. Transmission electron microscopy (TEM) has long been used to image dislocations in materials, and high-resolution electron microscopy can reveal dislocation core structures in high detail, particularly in annular dark-field mode. A TEM image, however, represents a two-dimensional projection of a three-dimensional (3D) object (although stereo TEM provides limited information about 3D dislocations). X-ray topography can image dislocations in three dimensions, but with reduced resolution. Using weak-beam dark-field TEM and scanning TEM, electron tomography has been used to image 3D dislocations at a resolution of about five nanometres (refs 15, 16). Atom probe tomography can offer higher-resolution 3D characterization of dislocations, but requires needle-shaped samples and can detect only about 60 per cent of the atoms in a sample. Here we report 3D imaging of dislocations in materials at atomic resolution by electron tomography. By applying 3D Fourier filtering together with equal-slope tomographic reconstruction, we observe nearly all the atoms in a multiply twinned platinum nanoparticle. We observed atomic steps at 3D twin boundaries and imaged the 3D core structure of edge and screw dislocations at atomic resolution. These dislocations and the atomic steps at the twin boundaries, which appear to be stress-relief mechanisms, are not visible in conventional two-dimensional projections. The ability to image 3D disordered structures such as dislocations at atomic resolution is expected to find applications in materials science, nanoscience, solid-state physics and chemistry.

In Situ Transmission Electron Microscopy of Lead Dendrites and Lead Ions in Aqueous Solution

An ideal technique for observing nanoscale assembly would provide atomic-resolution images of both the products and the reactants in real time. Using a transmission electron microscope we image in situ the electrochemical deposition of lead from an aqueous solution of lead(II) nitrate. Both the lead deposits and the local Pb(2+) concentration can be visualized. Depending on the rate of potential change and the potential history, lead deposits on the cathode in a structurally compact layer or in dendrites. In both cases the deposits can be removed and the process repeated. Asperities that persist through many plating and stripping cycles consistently nucleate larger dendrites. Quantitative digital image analysis reveals excellent correlation between changes in the Pb(2+) concentration, the rate of lead deposition, and the current passed by the electrochemical cell. Real-time electron microscopy of dendritic growth dynamics and the associated local ionic concentrations can provide new insight into the functional electrochemistry of batteries and related energy storage technologies.

Nanoscale temperature mapping in operating microelectronic devices

Plasmons can map temperature on the nanoscale Determining temperature on small length scales can be challenging: Direct probes can alter sample temperature, and radiation probes are limited by the wavelength of the light used. Mecklenberg et al. show how the bulk plasmon resonance of aluminum can be used to map the temperature on the nanoscale with transmission electron microscopy (see the Perspective by Colliex). Many other metals and semiconductors also have plasmon resonances that could also be used for temperature imaging. Science, this issue p. 629; see also p. 611 Electron microscopy measurement of the bulk plasmon of aluminum provides an accurate temperature probe. [Also see Perspective by Colliex] Modern microelectronic devices have nanoscale features that dissipate power nonuniformly, but fundamental physical limits frustrate efforts to detect the resulting temperature gradients. Contact thermometers disturb the temperature of a small system, while radiation thermometers struggle to beat the diffraction limit. Exploiting the same physics as Fahrenheit’s glass-bulb thermometer, we mapped the thermal expansion of Joule-heated, 80-nanometer-thick aluminum wires by precisely measuring changes in density. With a scanning transmission electron microscope and electron energy loss spectroscopy, we quantified the local density via the energy of aluminum’s bulk plasmon. Rescaling density to temperature yields maps with a statistical precision of 3 kelvin/hertz−1/2, an accuracy of 10%, and nanometer-scale resolution. Many common metals and semiconductors have sufficiently sharp plasmon resonances to serve as their own thermometers.

Allografts in Genetically Defined Rats: Difference in Survival between Kidney and Skin

Although skin allografts from inbred donors of the Fisher strain to inbred male Lewis recipients regularly show acute rejection within 12 days, orthotopic kidney allografts between untreated animals, in this same combination of strains, usually remain functionally intact for longer than 100 days. Since such renal allografts persist despite previous or concomitant rejection of skin allografts, neither acquired tolerance nor nonspecific immunosuppression can explain the surprisingly prolonged kidney survival. Many factors appear to be responsible for the disparate survival times observed. Tentatively, these factors are (i) antigenic differences between kidney and skin, (ii) intervention of immunological enhancement, and (iii) physiological differences in vulnerability between kidney and skin.

Imaging Nanobubbles in Water with Scanning Transmission Electron Microscopy

We present a technique based on scanning transmission electron microscopy (STEM) that is capable of probing nanobubble dynamics with nanometer spatial resolution. A vacuum-tight vessel holds a sub-micrometer layer of water between two electron-transparent dielectric membranes. Electrical current pulses passing through a platinum wire on one of the membranes inject sufficient heat locally to initiate single bubble formation. In the absence of power input, all bubbles are observed to be unstable against collapse, but the STEM beam alone can cause a shrinking bubble to grow.

Lithium-ion storage properties of titanium oxide nanosheets

A detailed kinetic analysis is used to determine the fundamental energy storage properties and rate capabilities of TiO2 nanosheets. These materials exhibit different properties compared to anatase nanocrystals including a shift to lower redox potentials for Li+ storage and the reversible charge storage of Na+. Nanosheets are intriguing for energy storage applications due to the fact that nearly the entire surface of the material, including specific crystal facets, can be exposed to the electrolyte.

Dark-field transmission electron microscopy and the Debye-Waller factor of graphene.

Graphenes structure bears on both the materials electronic properties and fundamental questions about long range order in two-dimensional crystals. We present an analytic calculation of selected area electron diffraction from multi-layer graphene and compare it with data from samples prepared by chemical vapor deposition and mechanical exfoliation. A single layer scatters only 0.5% of the incident electrons, so this kinematical calculation can be considered reliable for five or fewer layers. Dark-field transmission electron micrographs of multi-layer graphene illustrate how knowledge of the diffraction peak intensities can be applied for rapid mapping of thickness, stacking, and grain boundaries. The diffraction peak intensities also depend on the mean-square displacement of atoms from their ideal lattice locations, which is parameterized by a Debye-Waller factor. We measure the Debye-Waller factor of a suspended monolayer of exfoliated graphene and find a result consistent with an estimate based on the Debye model. For laboratory-scale graphene samples, finite size effects are sufficient to stabilize the graphene lattice against melting, indicating that ripples in the third dimension are not necessary.

Polarized light emission from individual incandescent carbon nanotubes

We fabricate nanoscale lamps which have a filament consisting of a single multiwalled carbon nanotube. After determining the nanotube geometry with a transmission electron microscope, we use Joule heating to bring the filament to incandescence, with peak temperatures in excess of 2000 K. We image the thermal light in both polarizations simultaneously as a function of wavelength and input electrical power. The observed degree of polarization is typically of the order of 75%, a magnitude predicted by a Mie model of the filament that assigns graphenes optical conductance

A one-step Cu/ZnO Quasi-Homogeneous Catalyst for DME Production from Syn-gas

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Simple phosphinate ligands access zinc clusters identified in the synthesis of zinc oxide nanoparticles

to each nanotube wall.