Ion implantation of graphene-toward IC compatible technologies.

Doping of graphene via low energy ion implantation could open possibilities for fabrication of nanometer-scale patterned graphene-based devices as well as for graphene functionalization compatible with large-scale integrated semiconductor technology. Using advanced electron microscopy/spectroscopy methods, we show for the first time directly that graphene can be doped with B and N via ion implantation and that the retention is in good agreement with predictions from calculation-based literature values. Atomic resolution high-angle dark field imaging (HAADF) combined with single-atom electron energy loss (EEL) spectroscopy reveals that for sufficiently low implantation energies ions are predominantly substitutionally incorporated into the graphene lattice with a very small fraction residing in defect-related sites.

STEM electron beam-induced current measurements of organic-inorganic perovskite solar cells.

We describe a new approach for preparing organic-inorganic perovskite solar cells for electron beam-induced current (EBIC) measurements in plan-view geometry. This method substantially reduces sample preparation artefacts, provides good electrical contact and keeps the preparation steps as close as possible to those for real devices. Our EBIC images were acquired simultaneously with annular dark-field scanning transmission electron microscopy images using a home-made highly sensitive EBIC amplifier. High-angle annular dark-field images and energy dispersive X-ray maps were recorded from the same area immediately afterwards. This allowed the EBIC contrast to be correlated with regions containing N and a deficiency of O. The EBIC contrast was also found to be similar to secondary electron contrast recorded with a scanning electron microscope. By identifying the generation and absorption electron processes, we determine that EBIC cannot be separated from the secondary electron and absorbed currents. This means that careful analysis needs to be performed before conclusions can be made on the origin of the current measured across p-n or p-i-n junctions.

Three-wave electron vortex lattices for measuring nanofields.

It is demonstrated how an electron-optical arrangement consisting of two electron biprisms can be used to generate three-wave vortex lattices with effective lattice spacings between 0.1 and 1 nm. The presence of vortices in these lattices was verified by using a third biprism to perform direct phase measurements via off-axis electron holography. The use of three-wave lattices for nanoscale electromagnetic field measurements via vortex interferometry is discussed, including the accuracy of vortex position measurements and the interpretation of three-wave vortex lattices in the presence of partial spatial coherence.

Tungsten disulphide sheathed carbon nanotubes.

An insulated nanotube wire is formed by the binary phase of layered tungsten disulphide and carbon nanotubes (shown in the HRTEM image) generated by the sulphidization of tungsten oxide coated multiwalled carbon nanotubes at 900 °C. Thermogravimetric analysis shows that the tungsten disulphide coat acts as an antioxidant.

The phonon contribution to high-resolution electron microscope images.

The amount of phonon scattering as a function of specimen thickness is determined for a clean silicon sample, free from amorphous surface layers, by measuring the diffuse scattering in energy-filtered convergent-beam diffraction patterns. It is found that for a 25 nm thick sample, only 7.5% of the intensity scattered to less than 18 nm(-1) is phonon scattered. This means that in a typical high-resolution sample most of the diffuse scattering is caused by surface amorphous layers rather than phonon scattering.

The contribution of phonon scattering to high-resolution images measured by off-axis electron holography.

The contribution of electrons that have been phonon scattered to the lattice fringe amplitude and the background intensity of a high-resolution electron microscope (HREM) image is addressed experimentally through the analysis of a defocus series of energy-filtered off-axis electron holograms. It is shown that at a typical specimen thickness used for HREM imaging approximately 15% of the electrons that contribute to an energy-filtered image have been phonon scattered. At this specimen thickness, the phonon-scattered electrons contribute a lattice image of opposite contrast to the elastic lattice image. The overall lattice fringe contrast is then reduced to 70% of the value that it would have in the absence of phonon scattering. At higher specimen thickness, the behaviour is defocus-dependent, with the phonon image having lattice fringe contrast of either the same or the opposite sense to the elastic image as the defocus is varied.

Atomic resolution imaging and spectroscopy of barium atoms and functional groups on graphene oxide.

We present an atomic resolution transmission electron microscopy (TEM) and scanning TEM (STEM) study of the local structure and composition of graphene oxide modified with Ba(2+). In our experiments, which are carried out at 80kV, the acquisition of contamination-free high-resolution STEM images is only possible while heating the sample above 400°C using a highly stable heating holder. Ba atoms are identified spectroscopically in electron energy-loss spectrum images taken at 800°C and are associated with bright contrast in high-angle annular dark-field STEM images. The spectrum images also show that Ca and O occur together and that Ba is not associated with a significant concentration of O. The electron dose used for spectrum imaging results in beam damage to the specimen, even at elevated temperature. It is also possible to identify Ba atoms in high-resolution TEM images acquired using shorter exposure times at room temperature, thereby allowing the structure of graphene oxide to be studied using complementary TEM and STEM techniques over a wide range of temperatures.

Hybridization approach to in-line and off-axis (electron) holography for superior resolution and phase sensitivity.

Holography--originally developed for correcting spherical aberration in transmission electron microscopes--is now used in a wide range of disciplines that involve the propagation of waves, including light optics, electron microscopy, acoustics and seismology. In electron microscopy, the two primary modes of holography are Gabor's original in-line setup and an off-axis approach that was developed subsequently. These two techniques are highly complementary, offering superior phase sensitivity at high and low spatial resolution, respectively. All previous investigations have focused on improving each method individually. Here, we show how the two approaches can be combined in a synergetic fashion to provide phase information with excellent sensitivity across all spatial frequencies, low noise and an efficient use of electron dose. The principle is also expected to be widely to applications of holography in light optics, X-ray optics, acoustics, ultra-sound, terahertz imaging, etc.

Comparison of approaches and artefacts in the measurement of detector modulation transfer functions.

In order to investigate the reproducibility of measurements of transmission electron microscope detector modulation transfer functions (MTFs) we measure the MTF of a charge-coupled device (CCD) camera using five different methods. MTFs derived from a sharp edge, a circular aperture and electron holographic interference fringes are found to agree closely with one other. The difficulty of obtaining accurate measurements of MTFs and the potential of using focused electron probes to make direct measurements of MTFs is discussed. We highlight the sensitivity of image contrast after deconvolution to small differences in the measured MTF.