Secondary-electron imaging of bulk crystalline specimens in an aberration corrected STEM.

Atomic-scale electron microscopy traditionally probes thin specimens, with thickness below 100 nm, and its feasibility for bulk samples has not been documented. In this study, we explore the practicality of scanning transmission electron microscope (STEM) imaging with secondary electrons (SE), using a silicon-wedge specimen having a maximum thickness of 18 µm. We find that the atomic structure is present in the entire thickness range of the SE images although the background intensity increases moderately with thickness. The consistent intensity of secondary electron (SE) images at atomic positions and the modest increase in background intensity observed in silicon suggest a limited contribution from SEs generated by backscattered electrons, a conclusion supported by our multislice calculations. We conclude that achieving atomic resolution in SE imaging for bulk specimens is indeed attainable using aberration-corrected STEM and an aberration-corrected scanning electron microscope (SEM) may have the capacity for atomic-level resolution, holding great promise for future strides in materials research.

NanoMi: An open source electron microscope hardware and software platform.

We outline a public license (open source) electron microscopy platform, referred to as NanoMi. NanoMi offers a modular, flexible electron microscope platform that can be utilized for a variety of applications, such as microscopy education and development of proof-of-principle experiments, and can be used to complement an existing experimental apparatus. All components are ultra-high vacuum compatible and the electron optics elements are independent from the vacuum envelope. The individual optical components are mounted on a 127 mm (5-inch) diameter half-pipe, allowing customizing of electron optics for a variety of purposes. The target capabilities include SEM, TEM, scanning TEM (STEM), and electron diffraction (ED) at up to 50 keV incident electron energy. The intended image resolution in SEM, TEM and STEM modes is ≈ 10 nm. We describe the existing components and the interfaces among components that ensure their compatibility and interchangeability. The paper provides a resource for those who consider building or utilizing their own NanoMi.

Phase plates in the transmission electron microscope: operating principles and applications.

In this paper, we review the current state of phase plate imaging in a transmission electron microscope. We focus especially on the hole-free phase plate design, also referred to as the Volta phase plate. We discuss the implementation, operating principles and applications of phase plate imaging. We provide an imaging theory that accounts for inelastic scattering in both the sample and in the hole-free phase plate.

Properties of Dipole-Mode Vibrational Energy Losses Recorded From a TEM Specimen.

The authors discuss the dipole vibrational modes that predominate in the energy-loss spectra of ionic materials below 1 eV, concentrating on thin-film specimens of typical transmission electron microscopy (TEM) thickness. The thickness dependence of the intensity is shown to be a useful guide to the bulk or surface character of vibrational peaks. The lateral and depth resolution of the energy-loss signal is investigated with the aid of finite-element calculations.

Thermal expansion coefficient measurement from electron diffraction of amorphous films in a TEM.

We measured the linear thermal expansion coefficients of amorphous 5-30 nm thick SiN and 17 nm thick Formvar/Carbon (F/C) films using electron diffraction in a transmission electron microscope. Positive thermal expansion coefficient (TEC) was observed in SiN but negative coefficients in the F/C films. In case of amorphous carbon (aC) films, we could not measure TEC because the diffraction radii required several hours to stabilize at a fixed temperature.

Bring your paper into the 'Fast Lane' of the editorial process and increase your changes for final acceptance in Micron, The International Research and Review Journal for Microscopy.

In the past few years Micron has revised the scope of the journal, bringing it back to its original core values when it was founded in 1969. Micron's aim is to be the leading international microscopy and microanalysis journal, covering the latest advances in the fields of biological and physical science. In order to achieve this, the editorial team carefully revised the guidelines to authors in 2011. As a team we now find it timely to report on the outcomes of this policy change.

Vibrational spectroscopy in the electron microscope.

Vibrational spectroscopies using infrared radiation, Raman scattering, neutrons, low-energy electrons and inelastic electron tunnelling are powerful techniques that can analyse bonding arrangements, identify chemical compounds and probe many other important properties of materials. The spatial resolution of these spectroscopies is typically one micrometre or more, although it can reach a few tens of nanometres or even a few ångströms when enhanced by the presence of a sharp metallic tip. If vibrational spectroscopy could be combined with the spatial resolution and flexibility of the transmission electron microscope, it would open up the study of vibrational modes in many different types of nanostructures. Unfortunately, the energy resolution of electron energy loss spectroscopy performed in the electron microscope has until now been too poor to allow such a combination. Recent developments that have improved the attainable energy resolution of electron energy loss spectroscopy in a scanning transmission electron microscope to around ten millielectronvolts now allow vibrational spectroscopy to be carried out in the electron microscope. Here we describe the innovations responsible for the progress, and present examples of applications in inorganic and organic materials, including the detection of hydrogen. We also demonstrate that the vibrational signal has both high- and low-spatial-resolution components, that the first component can be used to map vibrational features at nanometre-level resolution, and that the second component can be used for analysis carried out with the beam positioned just outside the sample--that is, for 'aloof' spectroscopy that largely avoids radiation damage.

Accurate measurement of relative tilt and azimuth angles in electron tomography: a comparison of fiducial marker method with electron diffraction.

Electron tomography is a method whereby a three-dimensional reconstruction of a nanoscale object is obtained from a series of projected images measured in a transmission electron microscope. We developed an electron-diffraction method to measure the tilt and azimuth angles, with Kikuchi lines used to align a series of diffraction patterns obtained with each image of the tilt series. Since it is based on electron diffraction, the method is not affected by sample drift and is not sensitive to sample thickness, whereas tilt angle measurement and alignment using fiducial-marker methods are affected by both sample drift and thickness. The accuracy of the diffraction method benefits reconstructions with a large number of voxels, where both high spatial resolution and a large field of view are desired. The diffraction method allows both the tilt and azimuth angle to be measured, while fiducial marker methods typically treat the tilt and azimuth angle as an unknown parameter. The diffraction method can be also used to estimate the accuracy of the fiducial marker method, and the sample-stage accuracy. A nano-dot fiducial marker measurement differs from a diffraction measurement by no more than ±1°.

Convenient contrast enhancement by a hole-free phase plate.

Decrease of the irradiation dose needed to obtain a desired signal-to-noise ratio can be achieved by Zernike phase-plate imaging. Here we present results on a hole-free phase plate (HFPP) design that uses the incident electron beam to define the center of the plate, thereby eliminating the need for high precision alignment and with advantages in terms of ease of fabrication. The Zernike-like phase shift is provided by a charge distribution induced by the primary beam, rather than by a hole in the film. Compared to bright-field Fresnel-mode imaging, the hole-free phase plate (HFPP) results in two- to four-fold increase in contrast, leading to a corresponding decrease in the irradiation dose required to obtain a desired signal-to-noise ratio. A local potential distribution, developed due to electron beam-induced secondary-electron emission, is the most likely mechanism responsible for the contrast-transfer properties of the HFPP.

Local thickness measurement through scattering contrast and electron energy-loss spectroscopy.

Scattering contrast measurements were performed on thin films of amorphous carbon and polycrystalline Au, as well as single-crystal MgO nanocubes. Based on the exponential absorption law, mass-thickness can be obtained within 10% accuracy by measuring the incident and transmitted intensities in the same image. For mass-thickness measurement of a thin amorphous specimen, a small collection semiangle improves the measurement sensitivity, whereas for the measurement of polycrystalline or single-crystal specimens, a large collection semiangle should be used to reduce diffraction-contrast effects. EELS thickness measurements on MgO nanocubes suggest that the Kramers-Kronig sum-rule method (with correction for plural and surface scattering) gives 10% accuracy at medium collection semiangles but overestimates the thickness at small collection semiangles, due to underestimation of the surface-mode scattering. The log-ratio method, with a formula for inelastic mean free path proposed by Malis et al. (1988), provides 10% accuracy at small collection semiangle, while that proposed by Iakoubovskii et al. (2008a) is preferable for medium and large collection semiangles. As a result of this work, we provide recommendations of preferred methods and conditions for local-thickness measurement in the TEM.

Water-soluble J-type rosette nanotubes with giant molar ellipticity.

A new self-assembling tricyclic module (×K1) featuring the Watson-Crick H-bonding arrays of guanine and cytosine fused to an internal pyridine ring was synthesized. When dissolved in water at room temperature, this module rapidly self-assembles into hexameric rosettes, which then stack to form J-type rosette nanotubes (RNTs) with increased inner/outer diameters and the largest molar ellipticity ever reported (4 × 10(6) deg·M(-1)·m(-1)). Using a combination of imaging and spectroscopic techniques we established the structure of ×K1-RNT and have shown that the extended π system of the self-assembling module resulted in a new family of J-type RNTs with enhanced intermodular electronic communication.

Heteroepitaxial growth of gold nanostructures on silicon by galvanic displacement.

This work focuses on the synthesis and interfacial characterization of gold nanostructures on silicon surfaces, including Si(111), Si(100), and Si nanowires. The synthetic approach uses galvanic displacement, a type of electroless deposition that takes place in an efficient manner under aqueous, room-temperature conditions. The case of gold-on-silicon has been widely studied and used for several applications and yet, a number of important, fundamental questions remain as to the nature of the interface. Some studies are suggestive of heteroepitaxial growth of gold on the silicon surface, whereas others point to the existence of a silicon-gold intermetallic sandwiched between the metallic gold and the underlying silicon substrate. Through detailed high resolution transmission electron microscopy (TEM), combined with selected area electron diffraction (SAED) and nanobeam diffraction (NBD), heteroepitaxial gold that is grown by galvanic displacement is confirmed on both Si(100) and Si(111), as well as silicon nanowires. The coincident site lattice (CSL) of gold-on-silicon results in a very small 0.2% lattice mismatch due to the coincidence of four gold lattices to three of silicon. The presence of gold-silicon intermetallics is suggested by the appearance of additional spots in the electron diffraction data. The gold-silicon interfaces appear heterogeneous with distinct areas of heteroepitaxial gold on silicon, and others, less well-defined, where intermetallics may reside. The high resolution cross-sectional TEM images reveal a roughened silicon interface under these aqueous galvanic displacement conditions, which most likely promotes nucleation of metallic gold islands that merge over time: a Volmer-Weber growth mechanism in the initial stages.

Fourier-ratio deconvolution techniques for electron energy-loss spectroscopy (EELS).

We discuss several ways of using Fourier-ratio deconvolution to process low-loss spectra. They include removal of the tail arising from the zero-loss peak, extraction of the spectrum of a particle from data recorded from the particle on a substrate, separation of the bulk and surface components in spectra recorded from samples of the same composition but different thickness, and investigation of interface energy-loss modes. We also demonstrate the use of a Bayesian-equivalent procedure based on the Richardson-Lucy algorithm.

Low-dose performance of parallel-beam nanodiffraction.

We evaluate the low-dose performance of parallel nano-beam diffraction (NBD) in the transmission electron microscope as a method for characterizing radiation sensitive materials at low electron irradiation dose. A criterion, analogous to Rose's, is established for detecting a diffraction spot with desired signal-to-noise ratio. Our experimental data show that a dose substantially lower than in high-resolution bright-field imaging is sufficient to determine structure and orientation of individual nanoscale objects embedded in amorphous matrix. In an instrument equipped with a cold field-emission gun it is possible to form a probe with sub-3 nm diameter and sub-0.3 mrad convergence angle with sufficient beam current to record a diffraction pattern with less than 0.2 s acquisition time. The interpretation of NBD patterns is identical to that of selected area diffraction patterns. We illustrate the physical principles underlying good low-dose performance of NBD by means of a phase grating. The electron irradiation dose needed to detect a diffraction peak in NBD is found proportional to 1/N2, where N is the number of lattice planes contributing to the peak.

Imaging of radiation-sensitive samples in transmission electron microscopes equipped with Zernike phase plates.

We have optimized a bright-field transmission electron microscope for imaging of high-resolution radiation-sensitive materials by calculating the imaging dose n(0) needed to obtain a signal-to-noise ratio (SNR)=5. Installing a Zernike phase plate (ZP) decreases the dose needed to detect single atoms by as much as a factor of two at 300 kV. For imaging larger objects, such as Gaussian objects with full-width at half-maximum larger than 0.15 nm, ZP appears more efficient in reducing the imaging dose than correcting for spherical aberration. The imaging dose n(0) does not decrease with extending of chromatic resolution limit by reducing chromatic aberration, using high accelerating potential (U(0)=300 kV), because the image contrast increases slower than the reciprocal of detection radius. However, reducing chromatic aberration would allow accelerating potential to be reduced leading to imaging doses below 10 e(-)/A(2) for a single iodine atom when a CS-corrector and a ZP are used together. Our simulations indicate that, in addition to microscope hardware, optimization is heavily dependent on the nature of the specimen under investigation.

Valence state map of iron oxide thin film obtained from electron spectroscopy imaging series.

This paper demonstrates the applicability of electron-spectroscopic imaging (ESI) for valence-state mapping of the iron oxide system. We have previously developed a set of signal-processing methods for an ESI series, to allow mapping of sp(2)/sp(3) ratio, dielectric function and energy bandgap. In this study, these methods are applied to generate a valence-state map of an iron oxide thin film (Fe/alpha-Fe(2)O(3)). Two problems, data undersampling and a convolution effect associated with extraction of the image-spectrum from the core loss image series, were overcome by using cubic-polynomial interpolation and maximum-entropy deconvolution. As a result, the reconstructed image-spectrum obtained from the ESI series images has a quality as good as that of conventional electron energy-loss spectra. The L(3)/L(2) ratio of the reconstructed ESI spectrum is determined to be 3.30+/-0.30 and 5.0+/-0.30 for Fe and alpha-Fe(2)O(3), respectively. Our L(3)/L(2) ratio mapping shows an accurate correspondence across the Cu/Fe/alpha-Fe(2)O(3) region. The effect of delocalization and chromatic aberration on the ESI resolution is discussed and estimated to be about 2 nm for the case of L(3)/L(2) ratio mapping.