We demonstrate a method to achieve high efficiency phase contrast imaging in aberration corrected scanning transmission electron microscopy (STEM) with a pixelated detector. The pixelated detector is used to record the Ronchigram as a function of probe position which is then analyzed with ptychography. Ptychography has previously been used to provide super-resolution beyond the diffraction limit of the optics, alongside numerically correcting for spherical aberration. Here we rely on a hardware aberration corrector to eliminate aberrations, but use the pixelated detector data set to utilize the largest possible volume of Fourier space to create high efficiency phase contrast images. The use of ptychography to diagnose the effects of chromatic aberration is also demonstrated. Finally, the four dimensional dataset is used to compare different bright field detector configurations from the same scan for a sample of bilayer graphene. Our method of high efficiency ptychography produces the clearest images, while annular bright field produces almost no contrast for an in-focus aberration-corrected probe.
The aberration-corrected scanning transmission electron microscope (STEM) has emerged as a key tool for atomic resolution characterization of materials, allowing the use of imaging modes such as Z-contrast and spectroscopic mapping. The STEM has not been regarded as optimal for the phase-contrast imaging necessary for efficient imaging of light materials. Here, recent developments in fast electron detectors and data processing capability is shown to enable electron ptychography, to extend the capability of the STEM by allowing quantitative phase images to be formed simultaneously with incoherent signals. We demonstrate this capability as a practical tool for imaging complex structures containing light and heavy elements, and use it to solve the structure of a beam-sensitive carbon nanostructure. The contrast of the phase image contrast is maximized through the post-acquisition correction of lens aberrations. The compensation of defocus aberrations is also used for the measurement of three-dimensional sample information through post-acquisition optical sectioning.
We observe interfacial ferromagnetism in superlattices of the paramagnetic metal LaNiO3 and the antiferromagnetic insulator CaMnO3. LaNiO3 exhibits a thickness dependent metal-insulator transition and we find the emergence of ferromagnetism to be coincident with the conducting state of LaNiO3. That is, only superlattices in which the LaNiO3 layers are metallic exhibit ferromagnetism. Using several magnetic probes, we have determined that the ferromagnetism arises in a single unit cell of CaMnO3 at the interface. Together these results suggest that ferromagnetism can be attributed to a double exchange interaction among Mn ions mediated by the adjacent itinerant metal.
Silicon (Si) nanoparticles embedded in a Mg 2 Si matrix (Mg 2 Si/xSi) have been successfully synthesized at 623 K from MgH 2 and Bi containing Si nanoparticle powders. The use of MgH 2 in this synthetic route avoids the formation of oxides through the generation of hydrogen and provides a route to homogeneously mixed Si nanoparticles within a doped Mg 2 Si matrix. The samples were characterized by powder X-ray diffraction, thermogravimetry/differential scanning calorimetry (TG/DSC), electron microprobe analysis (EMPA), and scanning transmission electron microscopy (STEM). The final crystallite size of Mg 2 Si obtained from the XRD patterns is about 50 nm for all the samples and the crystallite size of Si inclusions is approximately 17 nm. Theoretical calculations indicate that $5 mol% concentrations of Si nanoparticles with diameters in the 5-50 nm range could decrease the lattice thermal conductivity of Mg 2 Si by about 1-10% below the matrix value. Reduction in thermal conductivity was observed with the smallest amount of Si, 2.5 mol%. Larger amounts, x ¼ 10 mol%, did not provide any further reduction in thermal conductivity. Analysis of the microstructure of the Bi doped Mg 2 Si/xSi nanocomposites showed that the Bi dopant has a higher concentration at grain boundaries than within the grains and Bi preferentially substitutes the Mg site at the boundaries. The nanocomposite carrier concentration and mobility depend on the amount of Bi and Si inclusions in a complex fashion. Agglomerations of Si start to show up clearly in the Bi doped 5 mol% nanocomposite. While the inclusions result in a lower thermal conductivity, electrical resistivity and Seebeck are negatively affected as the presence of Si inclusions influences the amount of Bi dopant and therefore the carrier concentration. The x ¼ 2.5 mol% nanocomposite shows a consistently higher zT throughout the measured temperature range until the highest temperatures where a dimensionless figure of merit zT $ 0.7 was obtained at 775 K for Mg 2 Si/xSi with x ¼ 0 and 2.5 mol%. With optimization of the electronic states of the matrix and nanoparticle, further enhancement of the figure of merit may be achieved.
Screw dislocations play an important role in materials' mechanical, electrical and optical properties. However, imaging the atomic displacements in screw dislocations remains challenging. Although advanced electron microscopy techniques have allowed atomic-scale characterization of edge dislocations from the conventional end-on view, for screw dislocations, the atoms are predominantly displaced parallel to the dislocation line, and therefore the screw displacements are parallel to the electron beam and become invisible when viewed end-on. Here we show that screw displacements can be imaged directly with the dislocation lying in a plane transverse to the electron beam by optical sectioning using annular dark field imaging in a scanning transmission electron microscope. Applying this technique to a mixed [a+c] dislocation in GaN allows direct imaging of a screw dissociation with a 1.65-nm dissociation distance, thereby demonstrating a new method for characterizing dislocation core structures.
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