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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Atomic Scale Dynamics of Contact Formation in the Cross-Section of InGaAs Nanowire Channels

In the alloyed and compound contacts between metal and semiconductor transistor channels we see that they enable self-aligned gate processes which play a significant role in transistor scaling. At nanoscale dimensions and for nanowire channels, prior experiments focused on reactions along the channel length, but the early stage of reaction in their cross sections remains unknown. We report on the dynamics of the solid-state reaction between metal (Ni) and semiconductor (In 0.53 Ga 0.47 As), along the cross-section of nanowires that are 15 nm in width. Unlike planar structures where crystalline nickelide readily forms at conventional, low alloying temperatures, nanowires exhibit a solid-state amorphization step that can undergo a crystal regrowth step at elevated temperatures. Here, we capture the layer-by-layer reaction mechanism and growth rate anisotropy using in situ transmission electron microscopy (TEM). Our kinetic model depicts this new, in-plane contact formation which could pave the way for engineered nanoscale transistors.

36 MATERIALS SCIENCE↗
DOE OSTI2014

In-situ TEM observation of the response of ultrafine- and nanocrystalline-grained tungsten to extreme irradiation environments

The accumulation of defects, and in particular He bubbles, can have significant implications for the performance of materials exposed to the plasma in magnetic-confinement nuclear fusion reactors. Some of the most promising candidates for deployment into such environments are nanocrystalline materials as the engineering of grain boundary density offers the possibility of tailoring their radiation resistance properties. In order to investigate the microstructural evolution of ultrafine- and nanocrystalline-grained tungsten under conditions similar to those in a reactor, a transmission electron microscopy study with in situ 2 keV He1 ion irradiation at 9506C has been completed. A dynamic and complex evolution in the microstructure was observed including the formation of defect clusters, dislocations and bubbles. Nanocrystalline grains with dimensions less than around 60 nm demonstrated lower bubble density and greater bubble size than larger nanocrystalline (60–100 nm) and ultrafine (100–500 nm) grains. In grains over 100 nm, uniform distributions of bubbles and defects were formed. At higher fluences, large faceted bubbles were observed on the grain boundaries, especially on those of nanocrystalline grains, indicating the important role grain boundaries can play in trapping He and thus in giving rise to the enhanced radiation tolerance of nanocrystalline materials.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Structural and magnetic characterization of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles prepared via a facile microwave-assisted method

Nanoparticles of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO) with different particle sizes are synthesized by a very fast, inexpensive, reproducible, and environmentally friendly method: the microwave irradiation of the corresponding mixture of nitrates. The structural and magnetic properties of the samples are investigated by the X-Ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and magnetic (DC magnetization and AC susceptibility) measurements. The XRD study coupled with the Rietveld refinement show that all samples crystallize in a rhombohedral structure with the space group of R−3C. The FT-IR spectroscopy and FE-SEM images indicate formation of the perovskite structure of LSMO. The DC magnetization measurements confirm the decrease in the particle size effects on the magnetic properties, e.g. reduction in the ferromagnetic (FM) moment and increase in the surface spin disorder. Magnetic dynamics of the samples studied by AC magnetic susceptibility shows that the magnetic behavior of the nanometer-sized samples is well-described by the Vogel-Fulcher and critical slowing down laws. Strong interaction between magnetic nanoparticles of LSMO was detected by fitting the experimental data with the mentioned models. - Graphical abstract: Temperature dependence of the magnetization M(T) was measured in the zero-field-cooling (ZFC) and field-cooling (FC) modes at the applied magnetic field of 100 Oe for the La{sub 0.8}Sr{sub 0.2}MnO{sub 3} with different size prepared via a facile microwave-assisted method. - Highlights: • Nanoparticles of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} were synthesized by the microwave irradiation process. • The structural studies show that all samples crystallize in a rhombohedral structure with space group of R−3C. • The DC magnetic studies confirm tuning of the magnetic properties due to the particle size effects. • Magnetic dynamic studied by AC magnetic susceptibility indicate strong interaction between magnetic nanoparticles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Porosity Development at Li-Rich Layered Cathodes in All-Solid-State Battery during In Situ Delithiation

Structural evolutions are crucial for determining the performance of high-voltage lithium, manganese-rich layered cathodes. Moreover, interface between electrode and electrolyte plays a critical role in governing ionic transfer in all-solid-state batteries. In this work, we unveil two different types of porous structure in Li 1.2 Ni 0.2 Mn 0.6 O 2 cathode with LiPON solid-state electrolyte. Na-nopores are found near the cathode/electrolyte interface at pristine state, where cation mixing, phase transformation, oxygen loss and Mn reduction are also found. In situ Li + extraction induces the evolution of nanovoids, initially formed near the inter-face then propagated into the bulk. Despite the development of nanovoids, layered structure is conserved, suggesting the nature of nanopores and nanovoids are different and their impact would be divergent. This work demonstrates the intrinsic interfacial layer, as well as the dynamic scenario of nanovoid formation inside high-capacity layered cathode, which help understanding the performance fading in cathodes and offer insights into the all-solid-state battery design.

25 ENERGY STORAGE↗
DOE OSTI2020

Shape-preserving amorphous-to-crystalline transformation of CaCO3 revealed by in situ TEM

Organisms use inorganic ions and macromolecules to regulate crystallization from amorphous- precursors, endowing natural biominerals with complex morphologies and enhanced properties. The mechanisms by which modifiers enable these shape preserving transformations are poorly understood. We used in situ liquid-phase transmission electron microscopy to follow the evolution from amorphous calcium carbonate to calcite in the presence of additives. A combination of contrast analysis and infrared spectroscopy shows that Mg ions, which are widely present in seawater and biological fluids, alter the transformation pathway in a concentration-dependent manner. The ions bring excess (structural) water into the amorphous bulk so that a direct transformation is triggered by dehydration in the absence of morphological changes. Molecular dynamics simulations suggest Mg-incorporated water induces structural fluctuations, allowing transformation without the need to nucleate a separate crystal. Thus, the obtained calcite retains the original morphology of the amorphous state, biomimetically achieving the morphological control of crystals seen in biominerals

crystallization, biomineralization, calcium carbon↗
DOE OSTI2024

ELM-free enhanced D α H-mode with near zero NBI torque injection in DIII-D tokamak

Enhanced D α H-mode (EDA H-mode), an ELM-free H-mode regime, and the concomitant quasi-coherent mode (QCM) are explored in neutral beam heated, lower single null plasmas with near zero external torque injection. This regime exhibits good energy confinement (H 98y2 ~ 1) with β N ~ 2, high density, regime access at low input power, and no ELMs. New time–resolved measurements of electron and ion density, temperature, plasma rotation, and radial electric field as well as turbulence, flows, thermal and particle transport, and linear instability calculations examining the dynamics of the QCM are presented. Measurements using multiple fluctuation diagnostics reveal the QCM to be a separatrix spanning mode, peaking just inside the separatrix, existing in a wide range of k ⊥ ρ s ~ 0.1–1.2 with multiple harmonics, and propagating with a very small phase velocity in the plasma frame, where k ⊥ is the binormal wavenumber and ρ s is the ion sound radius. Linear gyrokinetic simulations of this EDA H-mode discharge with CGYRO indicate that the trapped electron mode (TEM) and electron temperature gradient mode are the dominant instabilities in the radial region where QCM is also unstable. Qualitative analysis indicates that the properties of TEM are consistent with the experimentally observed characteristics of the QCM. These similarities suggest that the QCM is consistent with a TEM instability existing in the edge region of the EDA H-mode plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Mechanical properties and deformation mechanisms of single crystal Mg micropillars subjected to high-strain-rate C-axis compression

Here, the mechanical properties and deformation mechanisms of single crystal magnesium under c-axis quasi-static and high-strain rate compressions are investigated through in situ scanning electron microscope (SEM) experiments and post-mortem transmission electron microscope (TEM) characterization. The findings revealed that ductility and high rates of hardening are preserved for pillars as large as 15 μm. Furthermore, rate effects result in a mild increase in flow stress with plastic deformations controlled primarily by the slip of type dislocations. Importantly and in contrast to other literature reports, plastic deformation occurs in the absence of twining. As the strain increases and plastic deformation exceeds about 4%, crystal rotation activates basal slip, <$\mathrm{a}$> type dislocations, resulting in a more rate independent flow stress. TEM observation on micropillars compressed at a strain rate of 250/s, revealed the activation of {${11}$$\bar{2}$$\bar{2}$} < $\bar{1}$$\bar{1}23$ > slip systems and high mobility of screw dislocations as major contributors to plastic strains in excess of 10% without fracture. These findings are relevant to the design of lightweight materials used in transportation systems, e.g., selection of material grain size. Moreover, the experimental data here reported provides the materials science community with a unique opportunity to validate discrete dislocation dynamics (DDD) formulations employed in multiscale design of materials.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Dielectric and ferroelectric properties of Pb{sub 0.88}La{sub 0.12}(Ti{sub 1−x}Mn{sub x}){sub 0.97}O{sub 3} nanoceramics

Graphical abstract: - Highlights: • The nanoceramics of La/Mn modified PbTiO{sub 3} are synthesized by mechano-thermal route. • Materials have been characterized using various experimental methods. • Drastic change in dielectric and electrical properties of PbTiO{sub 3} has been observed. • The high dielectric constant makes the material very promising candidate for DRAM. • The Mn substitution also makes the material useful for piezoelectric devices. - Abstract: The polycrystalline samples of Pb{sub 0.88}La{sub 0.12}(Ti{sub 1−x}Mn{sub x}){sub 0.97}O{sub 3} (x = 0.0, 0.04, 0.07, 0.10) (PLMT) were prepared using a mechano-thermal method. Preliminary structural analysis of the above samples, carried out using X-ray diffraction data, shows tetragonal structure. This study also shows that the basic compound PLT (Pb{sub 0.88}La{sub 0.12}TiO{sub 3}) retains its tetragonal structure even up to 10% of Mn substitution at the Ti-site. The transmission electron micrographs (TEM) of PLMT samples exhibit that materials prepared by the above method are found to be of nano-size. The temperature–frequency dependence of dielectric studies exhibits increase in relative permittivity with rise in Mn-concentration in PLMT, and hence it can make the materials useful for device applications. The temperature dependence of ac conductivity shows presence of different types of charge species. It is also observed that oxygen vacancies play a significant role in the high-temperature conduction-mechanism and dynamics of polarization of the system. Piezoelectric charge coefficient (d{sub 33}) increases with increase in the Mn content in PLMT.

36 MATERIALS SCIENCE↗
DOE OSTI2020

A pathway to synthesizing single-crystal Fe and FeCr films

Nuclear reactor environments provide a unique scientific and engineering challenge wherein materials must tolerate prolonged exposure to concurrent irradiation, elevated temperatures, and corrosive media. However, uncontrolled variability in material composition and structure often prohibits truly single-variable experiments that can reveal basic aspects of environmental damage. Here, Magnetron sputtering is used to provide a more controlled model system for these fundamental studies, yielding reproducible single-crystal Fe and FeCr thin films containing 8 and 18 at.% Cr. Electron microscopy is used to determine the systematic correlations between growth conditions and the resulting film microstructure and surface morphology. It is found that the substrate temperature and applied radio frequency (RF) bias can be tuned to obtain consistent homogeneous and single crystal films with a minimal amount of Ar impurities from the RF bias process. Epitaxial, single-crystal Fe films are obtained on MgO substrates at 500 °C with 10 Watt (W) RF bias deposition. However, when Cr is alloyed with Fe, higher substrate temperatures (600 °C) and applied RF biases (15 W) are required to achieve a similar epitaxial single-crystal FeCr film. Accelerated molecular dynamics simulations reveal that Cr impedes surface transport, explaining the need for higher temperature and bias during the growth of the Cr-bearing films.

36 MATERIALS SCIENCE↗
NASA NTRS2020

Microstructural and Isotopic Constraints on WL Rim Formation

Coordinated microanalyses of Wark-Lovering (WL) rims are needed to best understand their origin and to decipher their subsequent evolution both in the nebular and parent body settings. Here we present the mineralogy, petrology, microstructures, O isotopic compositions, and Al-Mg systematics of a WL rim on a Type B CAI, ‘‘Big Guy”, from the reduced CV3 chondrite Vigarano [1]. Our SEM and TEM study reveals seven distinct mineral layers in the WL rim that include: (1) gehlenite with rare grossite, (2) hibonite, (3) spinel with minor hibonite and perovskite, (4) zoned melilite (Åk(sub ~0-10)), (5) anorthite, (6) zoned diopside grading outwards from Al,Ti-rich to Al,Tipoor, and (7) forsterite intergrown with diopside. We infer a two-stage history in which WL rim formation was initiated by flash melting and extensive evaporation of the original inclusion edge, followed by subsequent condensation under highly dynamic conditions. The outermost edge of the CAI mantle is mineralogically and texturally distinct compared to the underlying mantle that is composed of coarse, zoned melilite (Åk(sub ~10-60)) grains. The mantle edge contains finegrained gehlenite with hibonite and rare grossite that likely formed by rapid crystallization from a Ca,Al-rich melt produced during a flash vaporization event [2]. These gehlenite and hibonite layers are surrounded by successive layers of spinel, melilite, diopside, and forsterite, indicating their sequential gas-solid reactions onto hibonite. Anorthite occurs as a discontinuous layer that corrodes adjacent melilite and Al-diopside, and appears to have replaced them [3,4], probably even later than the forsterite layer formation. All the WL rim minerals analyzed using the JSC NanoSIMS 50L are 16O-rich (Δ17O ≈ −23‰), indicating their formation in an 16O-rich gas reservoir. Our data are in contrast with many CV CAIs that show heterogeneous Δ 17O values across their WL rims [5]. Our Al-Mg data obtained using the UCLA ims-1290 ion microprobe of the CAI interior and the WL rim define a well-correlated isochron with (26Al/27Al)(sub 0) = 4.94 × 10(exp −5), indicating their synchronous formation ≤5 × 10(exp 4) years after the canonical CAI value. In contrast, no 26Mg excesses are observed in the WL rim anorthite, which suggests its later formation or later isotopic resetting in an 16O-rich gas reservoir, after 26Al had decayed.

Han, J.↗
DOE OSTI2017

Deformation response of cube-on-cube and non-coherent twin interfaces in AgCu eutectic after dynamic plastic compression

For this research, Split-Hopkinson pressure bar dynamic compression experiments were conducted to determine the defect/interface interaction dependence on interface type, bilayer thickness and interface orientation with respect to the loading direction in the Ag-Cu eutectic system. Specifically, the deformation microstructure in alloys with either a cube-on-cube orientation relationship with {111} Ag ||{111} Cu interface habit planes or a twin orientation relationship with {$\overline{3}13$} Ag ||{$\overline{1}12$} Cu interface habit planes and with bilayer thicknesses of 500 nm, 1.1 µm and 2.2 µm were probed using TEM. The deformation was carried by dislocation slip and in certain conditions, deformation twinning. The twinning response was dependent on loading orientation with respect to the interface plane, bilayer thickness, and interface type. Twinning was only observed when loading at orientations away from the growth direction and decreased in prevalence with decreasing bilayer thickness. Twinning in Cu was dependent on twinning partial dislocations being transmitted from Ag, which only occurred for cube-on-cube interfaces. Lastly, dislocation slip and deformation twin transfer across the interfaces is discussed in terms of the slip transfer conditions developed for grain boundaries in FCC alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Thermal Shape Stability of fcc Metal Nanocrystals Synthesized with Faceted Nonequilibrium Shapes

Highly refined capabilities of the shape-controlled solution-phase synthesis of metal nanocrystals (NCs) allow the generation of NCs with faceted nonequilibrium shapes, which optimize properties for target applications such as catalysis and plasmonics. Often, for such applications and also for TEM analysis, the NCs are removed from the solution-phase environment. We explore the postsynthesis evolution of these metastable NCs in a high-vacuum TEM environment. Specifically, here we analyze their reshaping toward the equilibrium Wulff shapes mediated by surface diffusion, where such reshaping degrades the above-mentioned optimized properties. Typical sizes for these NCs range from 5 to 30 nm or 10 3 –10 6 atoms, and reshaping often occurs on the time scale of minutes for temperatures around, say, 400 °C. We discuss the development of predictive stochastic atomistic-level models for NC evolution with a realistic description of surface diffusion. These models, in contrast to Molecular Dynamics, can naturally address the relevant time and length scales for these systems. KMC simulation results for the stochastic models are described, focusing on the reshaping of slightly elongated nanorods and of mildly truncated octahedra and nanocubes. In addition, we review appropriate theoretical formulations for reshaping, which involves the nucleation and growth on 2D islands or layers on outer facets of the NC. We note the limitations of classical nucleation theory in some scenarios and demonstrate the successes of a more fundamental and general master equation-based analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

A highly efficient catalyst of palygorskite-supported manganese oxide for formaldehyde oxidation at ambient and low temperature: Performance, mechanism and reaction kinetics

A series of palygorskite-supported manganese oxide (MnO x /PG) catalysts were prepd. by a pptn. method using different manganese precursor. The as-prepared MnO x /PG catalysts were used to evaluate the catalytic oxidn. of HCHO and characterized by BET, XRD, TG, Raman spectroscopy, TEM, H 2 -TPR, XPS, and chemical titration. The results showed that the crystalline phase, distribution and Mn valence states of MnO x on the surface of PG depended on the precursors. Birnessite-type manganese oxide (δ-MnO 2 ) formed and uniformly coated on the surface of PG when potassium permanganate (PP) was used as the precursor. The MnO x /PG-PP catalyst showed the best catalytic activity for HCHO removal at low temp. among these catalysts and achieved complete HCHO conversion at 150 °C. More importantly, the dynamic single-pass removal efficiency of MnO x /PG-PP catalyst for ppm-level HCHO oxidn. was as high as 95% under high GHSV (300 L/g·h) at ambient temp. MnO x /PG-PP catalyst also exhibited excellent cycling stability and long-term activity at low and ambient temp. The kinetic results of MnO x /PG-PP catalyst showed that the oxidn. of HCHO followed the Mars-van Krevelen mechanism. The possible reaction pathway of HCHO oxidn. was proposed based on in situ DRIFTS and TPSR studies. The large sp. surface area, highly distributed active component, a high proportion of Mn 4+ species, and lattice oxygen content are responsible for the high catalytic activity of MnO x /PG-PP for oxidn. of formaldehyde. This work developed a natural mineral supported manganese oxide as an inexpensive and efficient catalyst for the purifn. of HCHO in industrial or indoor air environment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Dependence of the impurity transport on the dominant turbulent regime in ELM-y H-mode discharges on the DIII-D tokamak

Laser blow-off injections of aluminum and tungsten have been performed on the DIII-D tokamak to investigate the variation of impurity transport in a set of dedicated ion and electron heating scans with a fixed value of the external torque. The particle transport is quantified via the Bayesian inference method, which, constrained by a combination of a charge exchange recombination spectroscopy, soft X-ray measurements, and VUV spectroscopy provides a detailed uncertainty quantification of transport coefficients. Contrasting discharge phases with a dominant electron and ion heating reveal 3-fold drop in the impurity confinement time and order of magnitude increase in midradius impurity diffusion, when additional electron heating is applied. Further, the calculated stationary aluminum density profiles reverse from peaked in electron heated to hollow in the ion heated case, following a similar trend as electron and carbon density. Comparable values of a core diffusion have been observed for W and Al ions, while differences in the propagation dynamics of these impurities are attributed to pedestal and edge transport. Modeling of the core transport with non-linear gyrokinetics code CGYRO, significantly underpredicts the magnitude of the variation in Al transport. Diffusion increases 3-times steeper with additional electron heat flux and 10-times lower diffusion is observed in ion heated case than predicted by the modeling. Here, the CGYRO model quantitatively matches the increase of the Al diffusion when approaching the linear threshold for the transition from the ion temperature gradient (ITG) to trapped electron mode (TEM).

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2025

From Pollutant Removal to Renewable Energy: MoS2-Enhanced P25-Graphene Photocatalysts for Malathion Degradation and H2 Evolution

The widespread presence of pesticides—especially malathion—in aquatic environments presents a major obstacle to conventional remediation strategies, while the ongoing global energy crisis underscores the urgency of developing renewable energy sources such as hydrogen. In this context, photocatalytic water splitting emerges as a promising approach, though its practical application remains limited by poor charge carrier dynamics and insufficient visible-light utilization. Herein, we report the design and evaluation of a series of TiO2-based ternary nanocomposites comprising commercial P25 TiO2, reduced graphene oxide (rGO), and molybdenum disulfide (MoS2), with MoS2 loadings ranging from 1% to 10% by weight. The photocatalysts were fabricated via a two-step method: hydrothermal integration of rGO into P25 followed by solution-phase self-assembly of exfoliated MoS2 nanosheets. The composites were systematically characterized using X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DRS), and photoluminescence (PL) spectroscopy. Photocatalytic activity was assessed through two key applications: the degradation of malathion (20 mg/L) under simulated solar irradiation and hydrogen evolution from water in the presence of sacrificial agents. Quantification was performed using UV-Vis spectroscopy, gas chromatography–mass spectrometry (GC-MS), and thermal conductivity detection (GC-TCD). Results showed that the integration of rGO significantly enhanced surface area and charge mobility, while MoS2 served as an effective co-catalyst, promoting interfacial charge separation and acting as an active site for hydrogen evolution. Nearly complete malathion degradation (~100%) was achieved within two hours, and hydrogen production reached up to 6000 µmol g−1 h−1 under optimal MoS2 loading. Notably, photocatalytic performance declined with higher MoS2 content due to recombination effects. Overall, this work demonstrates the synergistic enhancement provided by rGO and MoS2 in a stable P25-based system and underscores the viability of such ternary nanocomposites for addressing both environmental remediation and sustainable energy conversion challenges.

Chemistry↗
DOE OSTI2020

Influence of Ag metal dispersion on the thermal conversion of ethanol to butadiene over Ag-ZrO 2 /SiO 2 catalysts

Atomistic scale models were developed and coupled with experimental investigation to deliver a functional understanding of catalytic activity and selectivity in the conversion of ethanol to 1,3-butadiene over Ag/ZrO 2 /SiO 2 . A detailed evaluation of the structural and electronic properties of the resultant catalyst models led to the identification of critical active sites of the catalyst. More importantly, the extent of Ag dispersion on the SiO 2 support and relative proximity to ZrO 2 were found to vary with the oxidation state of Ag and local coordination environment (Ag-O SiO2 ) allowing for critical control of ethanol conversion towards butadiene or ethylene. Simulations revealed that less dispersed or clustered Ag contain predominantly Ag 0 charge state and promote conversion of ethanol to ethylene. The well-dispersed Ag/ZrO 2 /SiO 2 catalyst instead contain a larger fraction of cationic Ag δ+ , and predominantly promote ethanol dehydrogenation and subsequent production of butadiene. The theoretical insights drawn were validated and confirmed experimentally using TEM, XRD and reactivity measurements demonstrating the effect of Ag dispersion on the selectivity of ethanol conversion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Towards time-resolved MicroED grid preparation using mix-and-inject gas dynamic virtual nozzles

Recent progress in gas dynamic virtual nozzle (GDVN) technologies in combination with high-brilliance synchrotron and X-ray free-electron lasers (XFELs) has allowed the visualization of protein dynamics in crystallo by mixing macromolecular protein crystals with a substrate using tunable mixing times on the order of milliseconds to seconds prior to serial X-ray diffraction data collection. This has become the method of choice for high-resolution structure determination of intermediate states. However, such experiments require large counts of crystals of proper sizes for high-resolution data collection, and premium beam times for screening efforts. Cryogenic microcrystal electron diffraction (MicroED) represents a complementary technique that may be a more accessible avenue for time-resolved nanocrystallography compared with serial X-ray diffraction experiments. MicroED can produce full diffraction datasets from just a few submicrometre-thick crystals, and the approach is more readily accessible, requiring standard cryogenic transmission electron microscopy (TEM) equipment available at many universities and institutes. Cryogenic MicroED, like other forms of cryo-EM, begins with rapidly freezing biological material on electron microscopy grids. In the case of MicroED, micro- to nano-crystals (<500 nm thick) are deposited onto electron microscopy grids and plunge-frozen for subsequent electron diffraction data collection. Here, we have incorporated GDVN technology developed originally for XFEL experiments into the freezing process as a first step towards time-resolved studies. We describe the limited deposition efficiency of the model MicroED protein proteinase K on TEM grids using GDVNs, preceding sample vitrification and successful MicroED data collection. We discuss both the initial results from such experiments and the methodological challenges in developing this approach into a reliable workflow for millisecond-to-second time-resolved structural studies of macromolecules. Our results promise a strategy to deposit crystals on grids using GDVNs and determine high-resolution structures by MicroED, constituting a first step towards development of time-resolved MicroED experiments.

MicroED↗