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Indium selenide, In 2 Se 3 , has recently attracted growing interest due to its remarkable properties, including room temperature ferroelectricity, outstanding photoresponsivity, and exotic in-plane ferroelectricity, which open up new regimes for next generation electronics. In 2 Se 3 also provides the important advantage of tuning the electrical properties of ultrathin layers with an external electrical and magnetic field, making it a potential platform to study novel two-dimensional physics. Yet, In 2 Se 3 has many different polymorphs, and it has been challenging to synthesize a single phase material, especially using scalable growth methods, as needed for technological applications. We recently reported the growth of twin-free ultrathin layers of In 2 Se 3 prepared by a diffusion driven molecular beam epitaxy approach, and twin-free Bi 2 Se 3 layers grown on these unique virtual substrates. In this paper, we use aberration-corrected scanning transmission electron microscopy to characterize the microstructure of these materials. We emphasize features of the In 2 Se 3 layer and In 2 Se 3 /InP interface which provide evidence for understanding the growth mechanism that leads to the twin-free and single phase In 2 Se 3 . We also show that this In 2 Se 3 layer provides an ideal substrate for growth of twin-free Bi 2 Se 3 with a nearly defect-free interface. This approach for growing high-quality twin-free single phase two-dimensional crystals using InP substrates is likely to be applicable to other technologically important materials., Competing Interests: The authors declare no competing financial interest., (© 2024 The Authors. Published by American Chemical Society.)

Layered carbides are fascinating compounds due to their enormous structural and chemical diversity, as well as their potential to possess useful and tunable functional properties. Their preparation, however, is challenging and forces synthesis scientists to develop creative and innovative strategies to access high-quality materials. One unique compound among carbides is Mo 2 Ga 2 C. Its structure is related to the large and steadily growing family of 211 MAX phases that crystallize in a hexagonal structure (space group P 6 3 / mmc ) with alternating layers of edge-sharing M 6 X octahedra and layers of the A -element. Mo 2 Ga 2 C also crystallizes in the same space group, with the difference that the A- element layer is occupied by two A -elements, here Ga, that sit right on top of each other (hence named "221" compound). Here, we propose that the Ga content in this compound is variable between 2:2, 2:1, and 2: ≤1 (and 2:0) Mo/Ga ratios. We demonstrate that one Ga layer can be selectively removed from Mo 2 Ga 2 C without jeopardizing the hexagonal P 6 3 / mmc structure. This is realized by chemical treatment of the 221 phase Mo 2 Ga 2 C with a Lewis acid, leading to the "conventional" 211 MAX phase Mo 2 GaC. Upon further reaction with CuCl 2 , more Ga is removed and replaced with Cu (instead of fully exfoliating into the Ga-free Mo 2 C T x MXene), leading to Mo 2 Ga 1- x Cu x C still crystallizing with space group P 6 3 / mmc , however, with a significantly larger c -lattice parameter. Furthermore, 211 Mo 2 GaC can be reacted with Ga to recover the initial 221 Mo 2 Ga 2 C. All three reaction pathways have not been reported previously and are supported by powder X-ray diffraction (PXRD), electron microscopy, X-ray spectroscopy, and density functional theory (DFT) calculations.

Off-axis electron holography has evolved into a powerful electron-microscopy-based technique for characterizing electromagnetic fields with nanometer-scale resolution. In this paper, we present a review of the application of off-axis electron holography to the quantitative measurement of electrostatic potentials and charge density distributions. We begin with a short overview of the theoretical and experimental basis of the technique. Practical aspects of phase imaging, sample preparation and microscope operation are outlined briefly. Applications of off-axis electron holography to a wide range of materials are then described in more detail. Finally, challenges and future opportunities for electron holography investigations of electrostatic fields and charge density distributions are presented., (Copyright © 2019. Published by Elsevier B.V.)

The development of novel nano-oxide spintronic devices would benefit greatly from interfacing with emergent phenomena at oxide interfaces. In this paper, we integrate highly spin-split ferromagnetic semiconductor EuO onto perovskite SrTiO 3 (001). A careful deposition of Eu metal by molecular beam epitaxy results in EuO growth via oxygen out-diffusion from SrTiO 3 . This in turn leaves behind a highly conductive interfacial layer through generation of oxygen vacancies. Below the Curie temperature of 70 K of EuO, this spin-polarized two-dimensional t 2g electron gas at the EuO/SrTiO 3 interface displays very large positive linear magnetoresistance (MR). Soft x-ray angle-resolved photoemission spectroscopy (SX-ARPES) reveals the t 2g nature of the carriers. First principles calculations strongly suggest that Zeeman splitting, caused by proximity magnetism and oxygen vacancies in SrTiO 3 , is responsible for the MR. This system offers an as-yet-unexplored route to pursue proximity-induced effects in the oxide two-dimensional t 2g electron gas.

The quantum anomalous Hall effect (QAHE) that emerges under broken time-reversal symmetry in topological insulators (TIs) exhibits many fascinating physical properties for potential applications in nanoelectronics and spintronics. However, in transition metal-doped TIs, the only experimentally demonstrated QAHE system to date, the QAHE is lost at practically relevant temperatures. This constraint is imposed by the relatively low Curie temperature ( T c ) and inherent spin disorder associated with the random magnetic dopants. We demonstrate drastically enhanced T c by exchange coupling TIs to Tm 3 Fe 5 O 12 , a high- T c magnetic insulator with perpendicular magnetic anisotropy. Signatures showing that the TI surface states acquire robust ferromagnetism are revealed by distinct squared anomalous Hall hysteresis loops at 400 K. Point-contact Andreev reflection spectroscopy confirms that the TI surface is spin-polarized. The greatly enhanced T c , absence of spin disorder, and perpendicular anisotropy are all essential to the occurrence of the QAHE at high temperatures.

The successful operation of rechargeable batteries relies on reliable insertion/extraction of ions into/from the electrodes. The battery performance and the response of the electrodes to such ion insertion and extraction are directly related to the spatial distribution of the charge and its dynamic evolution. However, it remains unclear how charge is distributed in the electrodes during normal battery operation. In this work, we have used off-axis electron holography to measure charge distribution during lithium ion insertion into a Ge nanowire (NW) under dynamic operating conditions. We discovered that the surface region of the Ge core is negatively charged during the core-shell lithiation of the Ge NW, which is counterbalanced by positive charge on the inner surface of the lithiated LixGe shell. The remainder of the lithiated LixGe shell is free from net charge, consistent with its metallic characteristics. The present work provides a vivid picture of charge distribution and dynamic evolution during Ge NW lithiation and should form the basis for tackling the response of these and related materials under real electrochemical conditions.

The mean inner potential (MIP) and inelastic mean free path (IMFP) of undoped ZnTe are determined using a combination of off-axis electron holography and convergent beam electron diffraction. The ZnTe MIP is measured to be 13.7±0.6 V, agreeing with previously reported simulations, and the IMFP at 200 keV is determined to be 46±2 nm for a collection angle of 0.75 mrad. Dynamical effects affecting holographic phase imaging as a function of incident beam direction for several common semiconductors are systematically studied and compared using Bloch wave simulations. These simulation results emphasize the need for careful choice of specimen orientation when carrying out quantitative electron holography studies in order to avoid erroneous phase measurements.

The development of non-volatile logic through direct coupling of spontaneous ferroelectric polarization with semiconductor charge carriers is nontrivial, with many issues, including epitaxial ferroelectric growth, demonstration of ferroelectric switching and measurable semiconductor modulation. Here we report a true ferroelectric field effect-carrier density modulation in an underlying Ge(001) substrate by switching of the ferroelectric polarization in epitaxial c-axis-oriented BaTiO3 grown by molecular beam epitaxy. Using the density functional theory, we demonstrate that switching of BaTiO3 polarization results in a large electric potential change in Ge. Aberration-corrected electron microscopy confirms BaTiO3 tetragonality and the absence of any low-permittivity interlayer at the interface with Ge. The non-volatile, switchable nature of the single-domain out-of-plane ferroelectric polarization of BaTiO3 is confirmed using piezoelectric force microscopy. The effect of the polarization switching on the conductivity of the underlying Ge is measured using microwave impedance microscopy, clearly demonstrating a ferroelectric field effect.

Polarization fields within InAs nanopillars with zincblende(ZB)/wurtzite(WZ) polytype stacking are quantified. The displacement of charged ions inside individual tetrahedra of WZ regions is measured at the atomic scale. The variations of spontaneous polarization along the interface normal are related to strain at interfaces of different polytypes. Thus, direct correlation between local atomic structure and electric properties is demonstrated., (© 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

The atomic arrangements of two types of InAs dislocation cores associated by a Z-shape faulted dipole are observed directly by aberration-corrected high-angle annular-dark-field imaging. Single unpaired columns of different atoms in a matrix of dumbbells are clearly resolved, with observable variations of bonding lengths due to excess Coulomb force from bare ions at the dislocation core. The corresponding geometric phase analysis provides confirmation that the dislocation cores serve as origins of strain field inversion while stacking faults maintain the existing strain status.

The development of aberration-corrected electron microscopes (ACEMs) has made it possible to resolve individual atomic columns ('dumbbells') with correct interatomic spacings in elemental and compound semiconductors. Thus, the latest generations of ACEMs should become powerful instruments for determining detailed structural arrangements at defects and interfaces in these materials. This paper provides a short overview of off-line ('software') and on-line ('hardware') ACEM techniques, with particular reference to characterization of elemental and compound semiconductors. Exploratory probe-corrected studies of ZnTe/InP and ZnTe/GaAs epitaxial heterostructures and interfacial defects are also described. Finally, some of the associated problems and future prospects are briefly discussed.

Homogeneous heterostructural wurtzite (WZ)/zincblende (ZB) junctions are successfully fabricated in ZnSe nanobelts. Polarity continuity across the ZB/WZ interface is demonstrated. The saw-tooth-like potential profile induced by spontaneous polarization across the WZ/ZB/WZ interfaces is identified directly at the nanoscale. The polarization-induced charge distribution across the homogeneous heterostructural interfaces is proposed as a viable alternative approach towards charge tailoring in semiconductor nanostructures., (Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Hole accumulation in Ge/Si core/shell nanowires (NWs) has been observed and quantified using off-axis electron holography and other electron microscopy techniques. The epitaxial [110]-oriented Ge/Si core/shell NWs were grown on Si (111) substrates by chemical vapor deposition through the vapor-liquid-solid growth mechanism. High-angle annular-dark-field scanning transmission electron microscopy images and off-axis electron holograms were obtained from specific NWs. The excess phase shifts measured by electron holography across the NWs indicated the presence of holes inside the Ge cores. Calculations based on a simplified coaxial cylindrical model gave hole densities of (0.4 ± 0.2) /nm(3) in the core regions.

Phase-shifting electron holography was used to reconstruct the object-wave function of high-spatial-frequency specimens of HgCdTe, and the requirements for precise measurements were investigated. Fresnel fringes due to the electrostatic biprism caused serious calculation errors during the phase-shifting reconstruction. Uniform interference fringes, obtained by adjusting the biprism voltage to cancel out the Fresnel fringes, were needed to minimize these errors. High-resolution holograms of a HgCdTe single crystal were recorded with coarse interference fringes and a high visibility of 65% and then used to reconstruct the atomic-scale object wave. Although the spatial resolution (0.25 nm) of the transmission electron microscope was worse than the separation (0.16 nm) between Hg (or Cd) and Te columns, the crystal polarity was determined from the aberration-corrected object wave.

The mean-free-paths for inelastic scattering of high-energy electrons (200 keV) for AlAs and GaAs have been determined based on a comparison of thicknesses as measured by electron holography and convergent-beam electron diffraction. The measured values are 77 +/- 4 nm and 67 +/- 4 nm for AlAs and GaAs, respectively. Using these values, the mean inner potentials of AlAs and GaAs were then determined, from a total of 15 separate experimental measurements, to be 12.1 +/- 0.7 V and 14.0 +/- 0.6 V, respectively. These latter measurements show good agreement with recent theoretical calculations within experimental error.

Phasic and tonic inhibitory currents of hippocampal pyramidal neurons exhibit distinct pharmacological properties. Picrotoxin and bicuculline methiodide inhibited both components, consistent with a role for GABAA receptors; however, gabazine, at a concentration that abolished miniature GABAergic inhibitory postsynaptic currents and responses to exogenous GABA, had no effect on tonic currents. Because all GABA-activated GABAA receptors in pyramidal neurons are gabazine-sensitive, it follows that tonic currents are not GABA-activated. Furthermore, picrotoxin-sensitive spontaneous single-channel events recorded from outside-out patches had the same chord conductance as GABA-activated channels and were gabazine-resistant. Therefore, we hypothesize that GABAA receptors, constitutively active in the absence of GABA, mediate tonic current; the failure of gabazine to block tonic current reflects a lack of negative intrinsic efficacy of the antagonist. We compared the negative efficacies of bicuculline and gabazine using the general anesthetic propofol to directly activate GABAA receptors native to pyramidal neurons or alpha1beta3gamma2 receptors recombinantly expressed in human embryonic kidney 293 cells. Propofol activated gabazine-resistant, bicuculline-sensitive currents when applied to either preparation. Although gabazine had negligible efficacy as an inhibitor of propofol-activated currents, it prevented inhibition by bicuculline, which acts as an inverse agonist inhibiting GABA-independent gating. Recombinant alpha1beta1/3gamma2 receptors also mediated agonist-independent tonic currents that were resistant to gabazine and inhibited by bicuculline. Thus, gabazine is a competitive antagonist with negligible negative efficacy and is therefore unable to inhibit GABAA receptors that are active in the absence of GABA because of either anesthetic or spontaneous gating. Moreover, spontaneously active GABAA receptors mediate gabazine-resistant tonic currents in pyramidal neurons.

We report on the application of off-axis electron holography and high-resolution TEM to study the crystal habits of magnetosomes and magnetic microstructure in two coccoid morphotypes of magnetotactic bacteria collected from a brackish lagoon at Itaipu, Brazil. Itaipu-1, the larger coccoid organism, contains two separated chains of unusually large magnetosomes; the magnetosome crystals have roughly square projections, lengths up to 250 nm and are slightly elongated along [111] (width/length ratio of about 0.9). Itaipu-3 magnetosome crystals have lengths up to 120 nm, greater elongation along [111] (width/length approximately 0.6), and prominent corner facets. The results show that Itaipu-1 and Itaipu-3 magnetosome crystal habits are related, differing only in the relative sizes of their crystal facets. In both cases, the crystals are aligned with their [111] elongation axes parallel to the chain direction. In Itaipu-1, but not Itaipu-3, crystallographic positioning perpendicular to [111] of successive crystals in the magnetosome chain appears to be under biological control. Whereas the large magnetosomes in Itaipu-1 are metastable, single-magnetic domains, magnetosomes in Itaipu-3 are permanent, single-magnetic domains, as in most magnetotactic bacteria.

Wedge polishing was used to prepare one-dimensional Si n-p junction and Si p-channel metal-oxide-silicon field effect transistor (pMOSFET) samples for precise and quantitative electrostatic potential analysis using off-axis electron holography. To avoid artifacts associated with ion milling, cloth polishing with 0.02-microm colloidal silica suspension was used for final thinning. Uniform thickness and no significant charging were observed by electron holography analysis for samples prepared entirely by this method. The effect of sample thickness was investigated and the minimum thickness for reliable results was found to be approximately 160 nm. Below this thickness, measured phase changes were smaller than expected. For the pMOSFET sample, quantitative analysis of two-dimensional electrostatic potential distribution showed that the metallurgical gate length (separation between two extension junctions) was approximately 54 nm, whereas the actual gate length was measured to be approximately 70 nm by conventional transmission electron microscopy. Thus, source and drain junction encroachment under the gate was 16 nm.

A reconstruction technique for off-axis electron holography not requiring Fourier transformation is presented. Background intensity and amplitude modulation recorded in a hologram are normalized using an envelope function, and a cosine-function image corresponding to interference fringes is retrieved from the hologram. A reconstructed phase image is then calculated from the retrieved cosine image. After phase unwrapping, the phases due to carrier frequency and Fresnel diffraction from the biprism are removed using a reference hologram, and the corrected phase image is obtained. One advantage of this method is that the spatial resolution does not rely on the interference fringe spacing. Another advantage is that the phase image has no artifacts due to windowing of the sideband, which occurs in the usual Fourier-transformation method. Details of the calculation process and demonstrations of the method using a latex sphere particle and self-assembled Co nanoparticles are described.

The three-dimensional (3D) morphology of a nanometer-sized object can be obtained using electron tomography. Variations in composition or density of the object cause variations in the reconstructed intensity. When imaging homogeneous objects, variations in reconstructed intensity are caused by the imaging technique, imaging conditions, and reconstruction. In this paper, we describe data acquisition, image processing, and 3D reconstruction to obtain and compare tomograms of magnetite crystals from bright field (BF) transmission electron microscopy (TEM), annular dark-field (ADF) scanning transmission electron microscopy (STEM), and high-angle annular dark field (HAADF) STEM tilt series. We use histograms, which plot the number of volume elements (voxels) at a given intensity vs. the intensity, to measure and quantitatively compare intensity distributions among different tomograms. In combination with numerical simulations, we determine the influence of maximum tilt angle, tilt increment, contrast changes with tilt (diffraction contrast), and the signal-to-noise ratio (SNR) as well as the choice of the reconstruction approach (weighted backprojection (WB) and sequential iterative reconstruction technique (SIRT)) on the histogram. We conclude that because ADF and HAADF STEM techniques are less affected by diffraction, and because they have a higher SNR than BF TEM, they are better suited for tomography of nanometer-sized crystals.

A method for obtaining detailed two-dimensional strain maps in nanowires and related nanoscale structures has been developed. The approach relies on a combination of lattice imaging by high-resolution transmission electron microscopy and geometric phase analysis of the resulting micrographs using Fourier transform routines. We demonstrate the method for a germanium nanowire grown epitaxially on Si(111) by obtaining the strain components epsilon(xx), epsilon(yy), epsilon(xy), the mean dilatation, and the rotation of the lattice planes. The resulting strain maps are demonstrated to allow detailed evaluation of the strains and loading on nanowires.

High-resolution transmission electron microscopy and electron holography were used to study the habits of exceptionally large magnetite crystals in coccoid magnetotactic bacteria. In addition to the crystal habits, the crystallographic positioning of successive crystals in the magnetosome chain appears to be under strict biological control.

Quantitative analysis of electrostatic potential in semiconductor device samples using off-axis electron holography in the electron microscope is complicated by the presence of charged insulating layers. Preliminary results indicate that the behavior of p-type material near the Si-insulator interface may differ from that of n-type if the insulator is charging. Coating one side of the sample surface with carbon usually eliminates charging effects. Holographic phase measurements on thin silicon oxide film at liquid nitrogen temperature indicates that the maximum electric field near the edge of an charged region is 18 MV cm(-1), on the order of the breakdown voltage.

Off-axis electron holography is used to characterize a linear array of transistors, which was prepared for examination in cross-sectional geometry in the transmission electron microscope (TEM) using focused ion beam (FIB) milling from the substrate side of the semiconductor device. The measured electrostatic potential is compared with results obtained from TEM specimens prepared using the more conventional 'trench' FIB geometry. The use of carbon coating to remove specimen charging effects, which result in electrostatic fringing fields outside 'trench' specimens, is demonstrated. Such fringing fields are not observed after milling from the substrate side of the device. Analysis of the measured holographic phase images suggests that the electrically inactive layer on the surface of each FIB-milled specimen typically has a thickness of 100 nm.

We describe the synthesis of novel monocrystalline FeCo nanowires encapsulated inside multiwalled carbon nanotubes (MWNTs). These FeCo nanowires exhibit homogeneous Fe and Co concentrations and do not contain an external oxide layer due to the presence of insulating nanotube layers. The method involves the aerosol thermolysis of toluene-ferrocene-cobaltocene solutions in inert atmospheres. The materials have been carefully characterized using state-of-the-art high-resolution transmission electron microscopy (HRTEM), electron-energy-loss spectroscopy (EELS), scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDX), electron diffraction, HREELS-STM elemental mapping, X-ray powder diffraction, and SQUID magnetometry. We noted that the formation of FeCo alloys occurs at relatively low pyrolytic temperatures (e.g., 650-750 degrees C). These single-crystal nanowires, which have not been reported hitherto, always exhibit the FeCo (110) plane parallel to the carbon nanotube axis. The FeCo nanomaterials have shown large coercive fields at room temperature (e.g., 900 Oe). We envisage that these aligned ferromagnetic nanowires could be used in the fabrication of high-density magnetic storage devices and magnetic composites.

The Gerchberg-Papoulis (GP) iterative algorithm is applied to electron holographic reconstruction to supplement the Fourier-transform method. The GP algorithm can recover the phase to high accuracy using simulated holograms. This method is useful when a region of known amplitude is present, such as a region of vacuum or uniform thickness. Modulations of the phase on the order of 0.1 rad can be corrected significantly using this algorithm.

Specimen charging may be one of the most significant factors that contribute to the high variability and generally low quality of images in cryo-electron microscopy. Understanding the nature of specimen charging can help in devising methods to reduce or even avoid its effects and thus improve the rate of data collection as well as the quality of the data. We describe a series of experiments that help to characterize the charging phenomenon, which has been termed the Berriman effect. The pattern of buildup and disappearance of the charge pattern has led to several suggestions for how to alleviate the effect. Experiments are described that demonstrate the feasibility of such charge mitigation.

During in situ transmission electron microscopy (TEM) field emission experiments, carbon nanotubes are observed to strongly diffract the imaging TEM electron beam. We demonstrate that this effect is identical to that of a standard electrostatic biprism. We also demonstrate that the nanotube biprism can be used to capture electron-holographic information.

Silicon wafers with a complex but known dopant profile were used to explore possible methods for improving the reliability of off-axis electron holography for quantitative determination of electrostatic potential profiles in doped semiconductor devices. The variability of results from nominally identical structures was attributed to local charging and associated external fields, forcing the development of a more robust approach to hologram analysis that incorporated an additional phase correction factor rather than rely on vacuum for phase flattening. Consistent results in close agreement with simulated profiles based on measured dopant distributions could then be obtained. Carbon coating was shown to be effective in reducing accumulation of charge caused by emission of secondary electrons. Overall, this work demonstrates that reliable potential profiles from unbiased samples should be obtainable on a routine basis provided that regions suitable for flattening of the phase profile can be identified.

In both human and rat tissues, complex patterns of transcripts are derived from the genes that encode the gamma-aminobutyric acid (GABA)(A) receptor epsilon subunit. An epsilon subunit transcript (approximately 3.6 kb) is expressed at relatively high levels in regions of the human brain and heart, but is not detected in most other major tissues. The encoded human epsilon subunit (epsilon (h)) confers distinctive properties to receptors into which it assembles. A distinct transcript of the gene (6.2 kb) is expressed abundantly in a variety of human tissues. This alternative transcript (ET2) appears to originate from within the epsilon subunit gene. It is possible that this transcript encodes a truncated subunit (epsilon (hS)), containing all of the transmembrane and intracellular domains. However, a combination of biochemical and electrophysiological analyses does not support this hypothesis. A distinct transcript of the epsilon subunit gene, encoding a large extracellular pro/glx domain, is expressed abundantly in rat and mouse brain. Functional analyses also failed to provide evidence for incorporation of this subunit (epsilon (rL)) into recombinant receptors. However, a shorter rat epsilon subunit (epsilon (r)), which lacks the pro/glx domain, conferred epsilon (h)-like properties to recombinant receptors, providing evidence for a functional rat epsilon subunit. In common with its human orthologue, incorporation of the epsilon (r) subunit into recombinant GABA(A) receptors confers several distinctive properties, including a reduced modulation by the anesthetic propofol and the appearance of spontaneous current.

Quantitative two-dimensional maps of electrostatic potential in device structures are obtained using off-axis electron holography with a spatial resolution of 6 nm and a sensitivity of 0.17 V. Estimates of junction depth and variation in electrostatic potential obtained by electron holography, process simulation, and secondary ion mass spectroscopy show close agreement. Measurement artifacts due to sample charging and surface "dead layers" do not need to be considered provided that proper care is taken with sample preparation. The results demonstrate that electron holography could become an effective method for quantitative 2D analysis of dopant diffusion in deep-submicron devices.