200 keV cold field emission source using carbon cone nanotip: Application to scanning transmission electron microscopy.

We report the use of a pyrolytic carbon cone nanotip as field emission cathode inside a modern 200 kV dedicated scanning transmission electron microscope. We show an unprecedented improvement in the probe current stability while maintaining all the fundamental properties of a cold field emission source such as a small angular current density together with a high brightness. We have also studied the influence of the low extraction voltage, as enabled by the nanosized apex of the cones, on the electron optics properties of the source that prevent the formation of a virtual beam cross-over of the gun. We have addressed this resolution-limiting issue by coming up with a new electron optical source design.

Differential phase-contrast dark-field electron holography for strain mapping.

Strain mapping is an active area of research in transmission electron microscopy. Here we introduce a dark-field electron holographic technique that shares several aspects in common with both off-axis and in-line holography. Two incident and convergent plane waves are produced in front of the specimen thanks to an electrostatic biprism in the condenser system of a transmission electron microscope. The interference of electron beams diffracted by the illuminated crystal is then recorded in a defocused plane. The differential phase recovered from the hologram is directly proportional to the strain in the sample. The strain can be quantified if the separation of the images due to the defocus is precisely determined. The present technique has the advantage that the derivative of the phase is measured directly which allows us to avoid numerical differentiation. The distribution of the noise in the reconstructed strain maps is isotropic and more homogeneous. This technique was used to investigate different samples: a Si/SiGe superlattice, transistors with SiGe source/drain and epitaxial PZT thin films.

Realization of a tilted reference wave for electron holography by means of a condenser biprism.

As proposed recently, a tilted reference wave in off-axis electron holography is expected to be useful for aberration measurement and correction. Furthermore, in dark-field electron holography, it is considered to replace the reference wave, which is conventionally diffracted in an unstrained object area, by a well-defined object-independent reference wave. Here, we first realize a tilted reference wave by employing a biprism placed in the condenser system above three condenser lenses producing a relative tilt magnitude up to 20/nm at the object plane (300kV). Paraxial ray-tracing predicts condenser settings for a parallel illumination at the object plane, where only one half of the round illumination disc is tilted relative to the optical axis without displacement. Holographic measurements verify the kink-like phase modulation of the incident beam and return the interference fringe contrast as a function of the relative tilt between both parts of the illumination. Contrast transfer theory including condenser aberrations and biprism instabilities was applied to explain the fringe contrast measurement. A first dark-field hologram with a tilted - object-free - reference wave was acquired and reconstructed. A new application for bright/dark-field imaging is presented.

Development of splitting convergent beam electron diffraction (SCBED).

Using a combination of condenser electrostatic biprism with dedicated electron optic conditions for sample illumination, we were able to split a convergent beam electron probe focused on the sample in two half focused probes without introducing any tilt between them. As a consequence, a combined convergent beam electron diffraction pattern is obtained in the back focal plane of the objective lens arising from two different sample areas, which could be analyzed in a single pattern. This splitting convergent beam electron diffraction (SCBED) pattern has been tested first on a well-characterized test sample of Si/SiGe multilayers epitaxially grown on a Si substrate. The SCBED pattern contains information from the strained area, which exhibits HOLZ lines broadening induced by surface relaxation, with fine HOLZ lines observed in the unstrained reference part of the sample. These patterns have been analyzed quantitatively using both parts of the SCBED transmitted disk. The fine HOLZ line positions are used to determine the precise acceleration voltage of the microscope while the perturbed HOLZ rocking curves in the stained area are compared to dynamical simulated ones. The combination of these two information leads to a precise evaluation of the sample strain state. Finally, several SCBED setups are proposed to tackle fundamental physics questions as well as applied materials science ones and demonstrate how SCBED has the potential to greatly expand the range of applications of electron diffraction and electron holography.

Determining the work function of a carbon-cone cold-field emitter by in situ electron holography.

Cold-field emission properties of carbon cone nanotips (CCnTs) have been studied in situ in the transmission electron microscope (TEM). The current as a function of voltage, i(V), was measured and analyzed using the Fowler-Nordheim (F-N) equation. Off-axis electron holography was employed to map the electric field around the tip at the nanometer scale, and combined with finite element modeling, a quantitative value of the electric field has been obtained. For a tip-anode separation distance of 680 nm (measured with TEM) and a field emission onset voltage of 80 V, the local electric field was 2.55 V/nm. With this knowledge together with recorded i(V) curves, a work function of 4.8±0.3 eV for the CCnT was extracted using the F-N equation.

Study of nanocrystalline BiMnO3-PbTiO3: synthesis, structural elucidation, and magnetic characterization of the whole solid solution.

In the last ten years, the study and the search for new multiferroic materials have been a major challenge due to their potential applications in electronic technology. In this way, bismuth-containing perovskites (BiMO(3)), and particularly those in which the metal M position is occupied by a magnetically active cation, have been extensively investigated as possible multiferroic materials. From the point of view of synthesis, only a few of the possible bismuth-containing perovskites can be prepared by conventional methods but at high pressures. Herein, the preparation of one of these potential multiferroic systems, the solid solution xBiMnO(3)-(1-x)PbTiO(3) by mechanosynthesis is reported. Note that this synthetic method allows the oxides with high x values, and more particularly the BiMnO(3) phase, to be obtained as nanocrystalline phases, in a single step and at room temperature without the application of external pressure. These results confirm that, in the case of Bi perovskites, mechanosynthesis is a good alternative to high-pressure synthesis. These materials have been studied from the point of view of their structural characteristics by precession electron diffraction and magnetic property measurements.

A new linear transfer theory and characterization method for image detectors. Part II: experiment.

A novel generalized linear transfer theory describing the signal and noise transfer in image detectors has been developed in Part I (Niermann, this issue, [1]) of this paper. Similar to the existing notion of a point spread function (PSF) describing the transfer of the first statistical moment (the average), a noise spread function (NSF) was introduced to characterize the spatially resolved transfer of noise (central second moment, covariance). Following the theoretic results developed in Part I (Niermann, this issue, [1]), a new experimental method based on single spot illumination has been developed and applied to measure 2D point and 4D noise spread functions of CCD cameras used in TEM. A dedicated oversampling method has been used to suppress aliasing in the measured quantities. We analyze the 4D noise spread with respect to electronic and photonic noise contributions.

Nanoscale holographic interferometry for strain measurements in electronic devices.

Strained silicon is now an integral feature of the latest generation of transistors and electronic devices because of the associated enhancement in carrier mobility. Strain is also expected to have an important role in future devices based on nanowires and in optoelectronic components. Different strategies have been used to engineer strain in devices, leading to complex strain distributions in two and three dimensions. Developing methods of strain measurement at the nanoscale has therefore been an important objective in recent years but has proved elusive in practice: none of the existing techniques combines the necessary spatial resolution, precision and field of view. For example, Raman spectroscopy or X-ray diffraction techniques can map strain at the micrometre scale, whereas transmission electron microscopy allows strain measurement at the nanometre scale but only over small sample areas. Here we present a technique capable of bridging this gap and measuring strain to high precision, with nanometre spatial resolution and for micrometre fields of view. Our method combines the advantages of moiré techniques with the flexibility of off-axis electron holography and is also applicable to relatively thick samples, thus reducing the influence of thin-film relaxation effects.

Direct mapping of strain in a strained silicon transistor by high-resolution electron microscopy.

Aberration-corrected high-resolution transmission electron microscopy (HRTEM) is used to measure strain in a strained-silicon metal-oxide-semiconductor field-effect transistor. Strain components parallel and perpendicular to the gate are determined directly from the HRTEM image by geometric phase analysis. Si80Ge20 source and drain stressors lead to uniaxial compressive strain in the Si channel, reaching a maximum value of -1.3% just below the gate oxide, equivalent to 2.2 GPa. Strain maps obtained by linear elasticity theory, modeled with the finite-element method, agree with the experimental results to within 0.1%.