Electron diffraction analysis of individual single-walled carbon nanotubes

We present a detailed electron diffraction study of individual single-walled carbon nanotubes. A novel sample preparation procedure provides well-separated, long and straight individual single-shell nanotubes. Diffraction experiments are carried out at 60 kV, below the threshold for knock-on damage in carbon nanotubes. We describe experimental parameters that allow single-tube electron diffraction experiments with widely available thermal emission transmission electron microscopes. Further, we review the simulation of diffraction patterns for these objects.     

Effects of tilt on high-resolution ADF-STEM imaging

A study of the effects of small-angle specimen tilt on high-resolution annular dark field images was carried out for scanning transmission electron microscopes with uncorrected and aberration-corrected probes using multislice simulations. The results indicate that even in the cases of specimen tilts of the order of 1 degree a factor of 2 reduction in the contrast of the high-resolution image should be expected. The effect holds for different orientations of the crystal. Calculations also indicate that as the tilted specimen gets thicker the contrast reduction increases. Images simulated with a low-angle annular dark field detector show that tilt effects are more pronounced in this case and suggest that these low-angle detectors can be used to correct specimen tilt during scanning transmission electron microscopes operation.     

In situ TEM studies of local transport and structure in nanoscale multilayer films

This paper describes a novel technique for studying structure-transport correlations in nanoscale multilayer thin films. Here, local current-voltage characteristics from simplified magnetic tunnel junctions are measured in situ on cross-sectional transmission electron microscopy (TEM) samples and correlated directly with TEM images of the microstructure at the tunneling site. It is found that local variations in barrier properties can be detected by a point probe method, and that the tunneling barrier height and width can be extracted.     

Improvement of KFM performance by intermittent bias application method and by sampling detection of cantilever deflection

We have proposed an intermittent bias application method as well as a sampling detection method of cantilever deflection in Kelvin probe force microscopy (KFM) to improve its performances for surface potential measurements. In the former method, spiky biases, instead of the bias in a sinusoidal waveform normally used in KFM, are intermittently applied to generate electrostatic force at exact moments when the tip approaches the closest position to a sample surface. The latter one, on the other hand, realizes very sensitive detection of the electrostatic force, which is preferable in KFM. Both the dependence of the electrostatic force on the dc offset bias and the observed potential images clearly indicate that these two methods are very effective to improve the KFM performance.     

Determination of magnetic vortex polarity from a single Lorentz Fresnel image

Nanoscale confinement of the magnetization in a magnetic element often results in the creation of a vortex structure. The vortex equilibrium state is characterized by the curling of the in-plane magnetization (chirality) and an out-of-plane core magnetization. The polarity of the vortex core can point up or down, independent of the chirality, and, thus, magnetic elements with a vortex core are interesting as four-state logic elements. We present an easy-to-use, quantitative method for the determination of both chirality and polarity from a single Fresnel image. This method offers direct evidence of the three-dimensional structure of a magnetic vortex and has significant advantages over the more complex methods currently in use.     

Contact-resonance atomic force microscopy for nanoscale elastic property measurements: Spectroscopy and imaging

Quantitative measurements of the elastic modulus of nanosize systems and nanostructured materials are provided with great accuracy and precision by contact-resonance atomic force microscopy (CR-AFM). As an example of measuring the elastic modulus of nanosize entities, we used the CR-AFM technique to measure the out-of-plane indentation modulus of tellurium nanowires. A size-dependence of the indentation modulus was observed for the investigated tellurium nanowires with diameters in the range 20–150 nm. Over this diameter range, the elastic modulus of the outer layers of the tellurium nanowires experienced significant enhancement due to a pronounced surface stiffening effect. Quantitative estimations for the elastic moduli of the outer and inner parts of tellurium nanowires of reduced diameter are made with a core–shell structure model. Besides localized elastic modulus measurements, we have also developed a unique CR-AFM imaging capability to map the elastic modulus over a micrometer-scale area. We used this CR-AFM capability to construct indentation modulus maps at the junction between two adjacent facets of a tellurium microcrystal. The clear contrast observed in the elastic moduli of the two facets indicates the different surface crystallography of these facets.     

Extreme localization of electrons in space and time

Electron emission from sharp metal tips can take place on sub-femtosecond time scales if the emission is driven by few cycle femtosecond laser pulses. Here we outline the experimental prerequisites in detail, discuss emission regimes and relate them to recent experiments in the gas phase (attosecond physics). We present a process that leads to single atom tip emitters that are stable under laser illumination and conclude with a discussion of how to achieve short electron pulses at a target.     

An expanded approach to noise reduction from high-resolution STEM images based on the maximum entropy method

An expanded use of the maximum entropy method (MEM) is suggested to reduce noise from an experimental high-angle annular dark-field (HAADF) scanning transmission electron microscope (STEM) image. The MEM is combined with an estimate of the standard deviation of noise from an experimental HAADF STEM image and low-pass filtering using the information limit for an incoherent STEM image. Consequently, the present method has just one parameter of a Lagrange multiplier. It is demonstrated that the present method can reduce noise efficiently in high-resolution HAADF STEM images.     

Low temperature scanning electron microscopy: a review.

Low temperature scanning electron microscopy is useful for morphological and analytical studies both in situations where low temperature techniques are used during specimen preparation and where low temperature stages are used for specimen examination and analysis. Examples are given of different low temperature specimen preparation techniques and how they may be applied to different types of specimen. There are still a number of problems associated with morphological identification in fully frozen-hydrated samples and it is important to carry out parallel studies using more conventional transmission electron microscopy and light microscopy preparation techniques. A number of criteria are presented, some or all of which may be used to establish the existence of the frozen-hydrated state.     

Improved single neuron controller for multivariable stochastic systems with non-Gaussianities and unmodeled dynamics

In this paper, a new adaptive control approach is presented for multivariate nonlinear non-Gaussian systems with unknown models. A more general and systematic statistical measure, called (h,?)$(h,?)$-entropy, is adopted here to characterize the uncertainty of the considered systems. By using the “sliding window” technique, the non-parameter estimate of the (h,?)$(h,?)$-entropy is formulated. Then, the improved neuron based controllers are developed for multivariate nonlinear non-Gaussian systems by minimizing the entropies of the tracking errors in closed loops. The condition to guarantee the strictly decreasing entropy of tracking error is presented. Moreover, the convergence in the mean-square sense has been analyzed for all the weights in the neural controllers. Finally, the comparative simulation results are presented to show that the performance of the proposed algorithm is superior to that of PID control strategy.     

Optical and thermal processes involved in ultrafast laser pulse interaction with a field emitter

In the interaction between ultrafast laser pulses and a field emitter both optical and thermal processes are involved. In this paper, these physical process, and their timescales, are experimentally explored. Simple models are proposed to explain the observed experimental behaviour, and the influence of various parameters are investigated. In the case of optical processes, it is shown that the optical field is greatly enhanced at the tip apex, and that field evaporation could be induced by an optical non-linear effect called optical rectification. In the case of thermal processes, it is shown that the temperature rise because of light absorption can be determined and that the cooling process of the tip surface can be studied by pump probe measurements.     

Differential algebraic method for aberration analysis of typical electrostatic lenses

In this paper up to fifth-order geometric and third-order chromatic aberration coefficients of typical electrostatic lenses are calculated by means of the charged particle optics code, COSY INFINITY, based on the differential algebraic (DA) method. A two-tube immersion lens and a symmetric einzel lens have been chosen as two examples, whose axial potential distributions are numerically calculated by a FORTRAN program using the finite difference method. The DA results are in good agreement with those evaluated by the aberration integrals in electron optics. The DA method presented here can easily be extended to aberration analysis of other numerically computed electron lenses, including magnetic lenses.     

Image simulation of high resolution energy filtered TEM images

Inelastic image simulation software is presented, implementing the double channeling approximation which takes into account the combination of multiple elastic and single inelastic scattering in a crystal. The approach is described with a density matrix formalism. Two applications in high resolution energy filtered (EFTEM) transmission electron microscopy (TEM) images are presented: thickness-defocus maps for _SrTiO3${\mathrm{SrTiO}}_3$ and exit plane intensities for an (_LaAlO3)3(_SrTiO3)3$({\mathrm{LaAlO}}_3{)}_3({\mathrm{SrTiO}}_3{)}_3$ multilayer system. Both systems show a severe breakdown in direct interpretability which becomes worse for higher acceleration voltages, thicker samples and lower excitation edge energies. Since this effect already occurs in the exit plane intensity, it is a fundamental limit and image simulations in EFTEM are indispensable just as they are indispensable for elastic high resolution TEM images.     

Depth sectioning in scanning transmission electron microscopy based on core-loss spectroscopy

Recent and ongoing improvements in aberration correction have opened up the possibility of depth sectioning samples using the scanning transmission electron microscope in a fashion similar to the confocal scanning optical microscope. We explore questions of principle relating to image interpretability in the depth sectioning of samples using electron energy loss spectroscopy. We show that provided electron microscope probes are sufficiently fine and detector collection semi-angles are sufficiently large we can expect to locate dopant atoms inside a crystal. Furthermore, unlike high angle annular dark field imaging, electron energy loss spectroscopy can resolve dopants of smaller atomic mass than the supporting crystalline matrix.     

Kelvin force microscopy at the second cantilever resonance: an out-of-vacuum crosstalk compensation setup

We investigate the gap-voltage control loop in a Kelvin force microscopy setup with simultaneous non-contact topography imaging. The Kelvin controller electrostatically excites the second resonance of the cantilever at about 6.3 times the first resonance frequency and adjusts the DC component of the gap voltage to cancel the oscillation amplitude at this frequency, while the non-contact topography imaging is based on a frequency control loop that maintains a constant frequency of the mechanically excited first resonance of the cantilever by adjusting the tip-sample separation. Due to the self-excitation of the first resonance in our setup, it has to be considered that the electrostatic excitation at the second resonance frequency is applied to a closed feedback loop and cannot be considered as a simple superposition to the oscillation at the first resonance frequency. In particular, special care has to be taken about internal capacitive crosstalk between the tip bias and the cantilever deflection output signal. It is shown that such a coupling cannot be corrected by subtraction of a constant offset at the demodulator output since the crosstalk is sent into the self-excitation loop and is multiplied by the closed loop transfer function. We present a circuit that actively compensates, outside the vacuum environment, the internal crosstalk by adding to the deflection output a dephased fraction of the electrostatic excitation signal.     

Controlled environment vitrification system: An improved sample preparation technique

The controlled environment vitrification system (CEVS) permits cryofixation of hydrated biological and colloidal dispersions and aggregates from a temperature- and saturation-controlled environment. Otherwise, specimens prepared in an uncontrolled laboratory atmosphere are subject to evaporation and heat transfer, which may introduce artifacts caused by concentration, pH, ionic strength, and temperature changes. Moreover, it is difficult to fix and examine the microstructure of systems at temperatures other than ambient (e.g., biological systems at in vivo conditions and colloidal systems above room temperature). A system has been developed that ensures that a liquid or partially liquid specimen is maintained in its original state while it is being prepared before vitrification and, once prepared, is vitrified with little alteration of its microstructure. A controlled environment is provided within a chamber where temperature and chemical activity of volatile components can be controlled while the specimen is being prepared. The specimen grid is mounted on a plunger, and a synchronous shutter is opened almost simultaneously with the release of the plunger, so that the specimen is propelled abruptly through the shutter opening into a cryogenic bath. We describe the system and its use and illustrate the value of the technique with TEM micrographs of surfactant microstructures in which specimen preparation artifacts were avoided. We also discuss applications to other instruments like SEM, to other techniques like freeze-fracture, and to novel “on the grid” experiments that make it possible to freeze successive instants of dynamic processes such as membrane fusion, chemical reactions, and phase transitions.     

Loss of grain boundary segregant during ion milling

It is shown that material segregated to grain boundaries can be lost during ion milling. This specimen preparation artifact has been studied in the case of bismuth in copper and has also been observed for phosphorus in stainless steel. The loss is associated with specimen heating during ion milling and can be alleviated by good clamping and cooling of the specimen during milling. Specimen heating permits grain boundary diffusion of the segregating element to the specimen surfaces with subsequent loss of segregant from the specimen by evaporation or sputtering during ion milling. Loss of bismuth during in situ heating to 200–300°C is demonstrated. Therefore, care must be taken in specimen preparation for analytical electron microscopy measurement of such segregation. Similar effects may occur during ion milling of other materials, especially those where low thermal conductivity will result in high beam heating. In these cases, care must be taken to avoid loss of segregant during specimen preparation. Additional tests showed that no significant loss of segregant was observed during X-ray microanalysis, even at nominal room temperature and probe currents five-fold higher than that normally used for microanalysis.     

Artifacts introduced by ion milling in Al-Li-Cu alloys

Ion milling is commonly used to prepare specimens for observation under transmission electron microscope (TEM). This technique sometimes introduces artifacts in specimens contributing to misleading interpretation of TEM results as observed in the present investigation of Al-Li-Cu alloys. This type of alloy, in general, contains several kinds of precipitates, namely δ′ T₁, and θ′. It is found that ion milling even for a short time produces drastic changes in the precipitate characterics as compared to standard electropolishing methods of specimen preparation for TEM. Careful analysis of selected area diffraction patterns and micrographs shows that after ion milling δ′ precipitates are very irregular, whereas other precipitates coarsen and they are surrounded by misfit dislocations. In situ hot-stage TEM experiments were performed to relate the microstructure to that observed in the ion-milled specimen. Results and causes of ion milling effects on the microstructure are discussed in relation to standard electropolishing techniques and in situ hot-stage experiment.     

Towards better 3-D reconstructions by combining electron tomography and atom-probe tomography

Scanning transmission electron microscope tomography and atom-probe tomography are both three-dimensional techniques on the nanoscale. We demonstrate here the combination of the techniques by analyzing the very same volume of an Al-Ag alloy specimen. This comparison allows us to directly visualize the theoretically known artifacts of each technique experimentally, providing insight into the optimal parameters to use for reconstructions and assessing the quality of each reconstruction. The combination of the techniques for accurate morphology and compositional information in three dimensions at the nanoscale provides a route for a new level of materials characterization and understanding.     

Observation particle morphology of colloidal system by conventional SEM with an improved specimen preparation technique

On the basis of our previous report that polymer emulsion with different viscosity can be investigated by conventional scanning electron microscopy (SEM), we have developed an improved specimen preparation technique for obtaining particle morphology and size of colloidal silver, collagen, glutin, and polymer microspheres. In this study, we expect to provide a means for charactering the three-dimensional surface microstructure of colloidal particles. Dilution of the samples with appropriate volatile solvent like ethanol is effective for SEM specimen preparation. At a proper ratio between sample and ethanol, the colloidal particles are dispersed uniformly in ethanol and then deposited evenly on the substrate. Different drying methods are studied to search a proper drying condition, in which the small molecule solvent is removed without destroying the natural particle morphology. And the effects of ethanol in the specimen preparation process are described by analyzing the physicochemical properties of ethanol. The specimen preparation technique is simple and can be achieved in common laboratory for charactering the particle morphology of colloidal system.