89 research outputs found
Patterned probes for high precision 4D-STEM bragg measurements.
Nanoscale strain mapping by four-dimensional scanning transmission electron microscopy (4D-STEM) relies on determining the precise locations of Bragg-scattered electrons in a sequence of diffraction patterns, a task which is complicated by dynamical scattering, inelastic scattering, and shot noise. These features hinder accurate automated computational detection and position measurement of the diffracted disks, limiting the precision of measurements of local deformation. Here, we investigate the use of patterned probes to improve the precision of strain mapping. We imprint a "bullseye" pattern onto the probe, by using a binary mask in the probe-forming aperture, to improve the robustness of the peak finding algorithm to intensity modulations inside the diffracted disks. We show that this imprinting leads to substantially improved strain-mapping precision at the expense of a slight decrease in spatial resolution. In experiments on an unstrained silicon reference sample, we observe an improvement in strain measurement precision from 2.7% of the reciprocal lattice vectors with standard probes to 0.3% using bullseye probes for a thin sample, and an improvement from 4.7% to 0.8% for a thick sample. We also use multislice simulations to explore how sample thickness and electron dose limit the attainable accuracy and precision for 4D-STEM strain measurements
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Direct imaging of short-range order and its impact on deformation in Ti-6Al.
Chemical short-range order (SRO) within a nominally single-phase solid solution is known to affect the mechanical properties of alloys. While SRO has been indirectly related to deformation, direct observation of the SRO domain structure, and its effects on deformation mechanisms at the nanoscale, has remained elusive. Here, we report the direct observation of SRO in relation to deformation using energy-filtered imaging in a transmission electron microscope (TEM). The diffraction contrast is enhanced by reducing the inelastically scattered electrons, revealing subnanometer SRO-enhanced domains. The destruction of these domains by dislocation planar slip is observed after ex situ and in situ TEM mechanical testing. These results confirm the impact of SRO in Ti-Al alloys on the scale of angstroms. The direct confirmation of SRO in relationship to dislocation plasticity in metals can provide insight into how the mechanical behavior of concentrated solid solutions by the material's thermal history
Nanoscale mosaicity revealed in peptide microcrystals by scanning electron nanodiffraction.
Changes in lattice structure across sub-regions of protein crystals are challenging to assess when relying on whole crystal measurements. Because of this difficulty, macromolecular structure determination from protein micro and nanocrystals requires assumptions of bulk crystallinity and domain block substructure. Here we map lattice structure across micron size areas of cryogenically preserved three-dimensional peptide crystals using a nano-focused electron beam. This approach produces diffraction from as few as 1500 molecules in a crystal, is sensitive to crystal thickness and three-dimensional lattice orientation. Real-space maps reconstructed from unsupervised classification of diffraction patterns across a crystal reveal regions of crystal order/disorder and three-dimensional lattice tilts on the sub-100nm scale. The nanoscale lattice reorientation observed in the micron-sized peptide crystal lattices studied here provides a direct view of their plasticity. Knowledge of these features facilitates an improved understanding of peptide assemblies that could aid in the determination of structures from nano- and microcrystals by single or serial crystal electron diffraction
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In Situ TEM Study of the Degradation of PbSe Nanocrystals in Air
PbSe
nanocrystals have attracted widespread attention due to a
variety of potential applications. However, the practical utility
of these nanocrystals has been hindered by their poor air stability,
which induces undesired changes in the optical and electronic properties.
An understanding of the degradation of PbSe nanocrystals when they
are exposed to air is critical for improving the stability and enhancing
their applications. Here, we use in situ transmission electron microscopy
(TEM) with an environmental cell connected to air to study PbSe nanocrystal
degradation triggered by air exposure. We have also conducted a series
of complementary studies, including in situ environmental TEM study
of PbSe nanocrystals exposed to pure oxygen and PbSe nanocrystals
in H2O using a liquid cell, and ex situ experiments, such
as O2 plasma treatment and thermal heating of PbSe nanocrystals
under different air exposure. Our in situ observations reveal that
when PbSe nanocrystals are exposed to air (or oxygen) under electron
beam irradiation, they experience a series of changes, including shape
evolution of individual nanocrystals with the cuboid intermediates,
coalescence between nanocrystals, and formation of PbSe thin films
through drastic solid-state fusion. Further studies show that the
PbSe thin films transform into an amorphous Pb rich phase or eventually
pure Pb, which suggest that Se reacts with oxygen and can be evaporated
under electron beam illumination. These various in situ and ex situ
experimental results indicate that PbSe nanocrystal degradation in
air is initiated by the dissociation and removal of ligands from the
PbSe nanocrystal surface
Strong structural and electronic coupling in metavalent PbS moire superlattices
Moire superlattices are twisted bilayer materials, in which the tunable
interlayer quantum confinement offers access to new physics and novel device
functionalities. Previously, moire superlattices were built exclusively using
materials with weak van der Waals interactions and synthesizing moire
superlattices with strong interlayer chemical bonding was considered to be
impractical. Here using lead sulfide (PbS) as an example, we report a strategy
for synthesizing of moire superlattices coupled by strong chemical bonding. We
use water-soluble ligands as a removable template to obtain free-standing
ultra-thin PbS nanosheets and assemble them into direct-contact bilayers with
various twist angles. Atomic-resolution imaging shows the moire periodic
structural reconstruction at superlattice interface, due to the strong
metavalent coupling. Electron energy loss spectroscopy and theoretical
calculations collectively reveal the twist angle26 dependent electronic
structure, especially the emergent separation of flat bands at small twist
angles. The localized states of flat bands are similar to well-arranged quantum
dots, promising an application in devices. This study opens a new door to the
exploration of deep energy modulations within moire superlattices alternative
to van der Waals twistronics
Multiple generations of grain aggregation in different environments preceded solar system body formation
Manuscript submitted to Proceedings of the National Academy of ScienceThe solar system formed from interstellar dust and gas in a molecular cloud. Astronomical observations show that typical interstellar dust consists of amorphous (a-) silicate and organic carbon. Bona fide physical samples for laboratory studies would yield unprecedented insight about solar system formation, but they were largely destroyed. The most likely repositories of surviving presolar dust are the least altered extraterrestrial materials, interplanetary dust particles (IDPs) with probable cometary origins. Cometary IDPs contain abundant submicron a-silicate grains called GEMS, believed to be carbon-free. Some have detectable isotopically anomalous a-silicate components from other stars, proving they are preserved dust inherited from the interstellar medium. However, it is debated whether the majority of GEMS predate the solar system or formed in the solar nebula by condensation of high-temperature (>1300K) gas. Here, we map IDP compositions with single nanometer-scale resolution and find that GEMS contain organic carbon. Mapping reveals two generations of grain aggregation, the key process in growth from dust grains to planetesimals, mediated by carbon. GEMS grains, some with a-silicate subgrains mantled by organic carbon, comprise the earliest generation of aggregates. These aggregates (and other grains) are encapsulated in lower density organic carbon matrix, indicating a second generation of aggregation. Since this organic carbon thermally decomposes above ~450K, GEMS cannot have accreted in the hot solar nebula and formed, instead, in the cold presolar molecular cloud and/or outer protoplanetary disk. We suggest that GEMS are consistent with surviving interstellar dust, condensed in situ, and cycled through multiple molecular clouds.Portions of this work were performed at the Molecular Foundry and the Advanced Light Source at Lawrence Berkeley National Laboratory, which are supported by the Office of Science, Basic Energy Sciences, U.S. Department of Energy under Contract No. DE-AC02-05CH11231. HAI acknowledges funding by NASA’s Laboratory Analysis of Returned Samples and Emerging Worlds Programs (NNX14AH86G and NNX16AK41G). JPB acknowledges funding by NASA’s Cosmochemistry Program (NNX14AI39G). CF acknowledges funding by NASA’s Cosmochemistry Program (NNX14AG25G)
Strain fields in twisted bilayer graphene
Van der Waals heteroepitaxy allows deterministic control over lattice
mismatch or azimuthal orientation between atomic layers to produce long
wavelength superlattices. The resulting electronic phases depend critically on
the superlattice periodicity as well as localized structural deformations that
introduce disorder and strain. Here, we introduce Bragg interferometry, based
on four-dimensional scanning transmission electron microscopy, to capture
atomic displacement fields in twisted bilayer graphene with twist angles <
2{\deg}. Nanoscale spatial fluctuations in twist angle and uniaxial
heterostrain are statistically evaluated, revealing the prevalence of
short-range disorder in this class of materials. By quantitatively mapping
strain tensor fields we uncover two distinct regimes of structural relaxation
-- in contrast to previous models depicting a single continuous process -- and
we disentangle the electronic contributions of the rotation modes that comprise
this relaxation. Further, we find that applied heterostrain accumulates
anisotropically in saddle point regions to generate distinctive striped shear
strain phases. Our results thus establish the reconstruction mechanics
underpinning the twist angle dependent electronic behaviour of twisted bilayer
graphene, and provide a new framework for directly visualizing structural
relaxation, disorder, and strain in any moir\'e material.Comment: 29 pages, 6 figures plus supporting information (42 pages, 28
figures
Rotational and Dilational Reconstruction in Transition Metal Dichalcogenide Moir\'e Bilayers
Lattice reconstruction and corresponding strain accumulation play a key role
in defining the electronic structure of two-dimensional moir\'e superlattices,
including those of transition metal dichalcogenides (TMDs). Imaging of TMD
moir\'es has so far provided a qualitative understanding of this relaxation
process in terms of interlayer stacking energy, while models of the underlying
deformation mechanisms have relied on simulations. Here, we use interferometric
four-dimensional scanning transmission electron microscopy to quantitatively
map the mechanical deformations through which reconstruction occurs in
small-angle twisted bilayer MoS2 and WSe2/MoS2 heterobilayers. We provide
direct evidence that local rotations govern relaxation for twisted
homobilayers, while local dilations are prominent in heterobilayers possessing
a sufficiently large lattice mismatch. Encapsulation of the moir\'e layers in
hBN further localizes and enhances these in-plane reconstruction pathways,
suppressing out-of-plane corrugation. We also find that extrinsic uniaxial
heterostrain, which introduces a lattice constant difference in twisted
homobilayers, leads to accumulation and redistribution of reconstruction
strain, demonstrating another route to modify the moir\'e potential.Comment: 27 pages, 5 figure
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