scholarly journals Detection of isolated protein-bound metal ions by single-particle cryo-STEM

2017 ◽  
Vol 114 (42) ◽  
pp. 11139-11144 ◽  
Author(s):  
Nadav Elad ◽  
Giuliano Bellapadrona ◽  
Lothar Houben ◽  
Irit Sagi ◽  
Michael Elbaum
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Metal Ions ◽  
Single Particle ◽  
Dark Field ◽  
X Ray ◽  
X Ray Crystallography ◽  
Metal Atoms ◽  
Transmission Electron ◽  
Structural Methods

Metal ions play essential roles in many aspects of biological chemistry. Detecting their presence and location in proteins and cells is important for understanding biological function. Conventional structural methods such as X-ray crystallography and cryo-transmission electron microscopy can identify metal atoms on protein only if the protein structure is solved to atomic resolution. We demonstrate here the detection of isolated atoms of Zn and Fe on ferritin, using cryogenic annular dark-field scanning transmission electron microscopy (cryo-STEM) coupled with single-particle 3D reconstructions. Zn atoms are found in a pattern that matches precisely their location at the ferroxidase sites determined earlier by X-ray crystallography. By contrast, the Fe distribution is smeared along an arc corresponding to the proposed path from the ferroxidase sites to the mineral nucleation sites along the twofold axes. In this case the single-particle reconstruction is interpreted as a probability distribution function based on the average of individual locations. These results establish conditions for detection of isolated metal atoms in the broader context of electron cryo-microscopy and tomography.

scholarly journals Synthesis of nickel/gallium nanoalloys using a dual-source approach in 1-alkyl-3-methylimidazole ionic liquids

2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dual Source ◽  
Induced Decomposition

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.

scholarly journals Biosynthesized Highly Stable Au/C Nanodots: Ideal Probes for the Selective and Sensitive Detection of Hg2+ Ions

Nanomaterials ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 245 ◽  
Author(s):  
Sada Venkateswarlu ◽  
Saravanan Govindaraju ◽  
Roopkumar Sangubotla ◽  
Jongsung Kim ◽  
Min-Ho Lee ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Metal Ions ◽  
Fluorescent Probe ◽  
Photoelectron Spectroscopy ◽  
Industrial Development ◽  
Carbon Nanodots ◽  
Detection Mechanism ◽  
X Ray ◽  
Transmission Electron

The enormous ongoing industrial development has caused serious water pollution which has become a major crisis, particularly in developing countries. Among the various water pollutants, non-biodegradable heavy metal ions are the most prevalent. Thus, trace-level detection of these metal ions using a simple technique is essential. To address this issue, we have developed a fluorescent probe of Au/C nanodots (GCNDs-gold carbon nanodots) using an eco-friendly method based on an extract from waste onion leaves (Allium cepa-red onions). The leaves are rich in many flavonoids, playing a vital role in the formation of GCNDs. Transmission electron microscopy (TEM) and Scanning transmission electron microscopy-Energy-dispersive X-ray spectroscopy (STEM-EDS) elemental mapping clearly indicated that the newly synthesized materials are approximately 2 nm in size. The resulting GCNDs exhibited a strong orange fluorescence with excitation at 380 nm and emission at 610 nm. The GCNDs were applied as a fluorescent probe for the detection of Hg2+ ions. They can detect ultra-trace concentrations of Hg2+ with a detection limit of 1.3 nM. The X-ray photoelectron spectroscopy results facilitated the identification of a clear detection mechanism. We also used the new probe on a real river water sample. The newly developed sensor is highly stable with a strong fluorescent property and can be used for various applications such as in catalysis and biomedicine.

scholarly journals (Al,Mg)3La: a new phase in the Mg–Al–La system

2018 ◽  
Vol 74 (4) ◽  
pp. 370-375 ◽  
Author(s):  
Charlotte Wong ◽  
Mark J. Styles ◽  
Suming Zhu ◽  
Dong Qiu ◽  
Stuart D. McDonald ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Powder Diffraction ◽  
Dark Field ◽  
Transmission Electron Microscopy Analysis ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Electron Microscopy Analysis

During an investigation of the Mg-rich end of the Mg–Al–La system, a new ternary phase with the composition of (Al,Mg)3La was identified. The crystal structure of this phase was determined by conventional X-ray powder diffraction and transmission electron microscopy analysis and refined using high-resolution X-ray powder diffraction. The (Al,Mg)3La phase is found to have an orthorhombic structure with a space group of C2221 and lattice parameters of a = 4.3365 (1) Å, b = 18.8674 (4) Å and c = 4.4242 (1) Å, which is distinctly different from the binary Al3La phase (P63/mmc). The resolved structure of the (Al,Mg)3La phase is further verified by high-angle annular dark-field scanning transmission electron microscopy.

scholarly journals In Situ Ternary Boride: Effects on Densification Process and Mechanical Properties of WC-Co Composite Coating

Materials ◽  
2020 ◽  
Vol 13 (8) ◽  
pp. 1995
Author(s):  
Junfeng Bao ◽  
Yueguang Yu ◽  
Bowen Liu ◽  
Chengchang Jia ◽  
Chao Wu
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Transmission Electron Microscopy ◽  
Bonding Strength ◽  
Dark Field ◽  
Flame Spraying ◽  
Composite Powders ◽  
X Ray ◽  
Transmission Electron ◽  
Ternary Boride

New coatings resistant to corrosion in high-temperature molten zinc aluminum were prepared by supersonic flame spraying of various composite powders. These composite powders were prepared by mixing, granulation, and heat treatment of various proportions of Mo–B4C powder and WC and Co powder. X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), high-angle annular dark-field scanning transmission electron microscopy (HAADF–STEM), energy dispersive X-ray spectroscopy (EDS), and mechanical analysis were used to study the effects of Mo–B4C on the microstructure, phase, porosity, bonding strength, and elastic modulus of the composite powder and coating. Results show that the addition of an appropriate quantity of Mo–B4C reacts with Co to form ternary borides CoMo2B2 and CoMoB. Ternary boride forms a perfect continuous interface, improving the mechanical properties and corrosion resistance property of the coating. When the amount of Mo–B4C added was 35.2%, the mechanical properties of the prepared coating reached optimal values: minimum porosity of 0.31 ± 0.15%, coating bonding strength of 77.81 ± 1.77 MPa, nanoindentation hardness of 20.12 ± 1.85 GPa, Young’s modulus of 281.52 ± 30.22 GPa, and fracture toughness of 6.38 ± 0.45 MPa·m1/2.

Effect of using polyimide capillaries during thermal experiments on the particle size distribution of supported Pt nanoparticles

2015 ◽  
Vol 48 (5) ◽  
pp. 1599-1603 ◽  
Author(s):  
Liliana Gámez-Mendoza ◽  
Oscar Resto ◽  
María Martínez-Iñesta
Keyword(s):  
Electron Microscopy ◽  
Thermal Stability ◽  
Transmission Electron Microscopy ◽  
Low Cost ◽  
Pt Nanoparticles ◽  
Dark Field ◽  
High Angle ◽  
X Ray ◽  
Transmission Electron ◽  
Annular Dark Field

Kapton HN-type polyimide capillaries are commonly used as sample holders for transmission X-ray experiments at temperatures below 673 K because of their thermal stability, high X-ray transmittance and low cost. Using high-angle annular dark field scanning high-resolution transmission electron microscopy and thermogravimetric analysis, this work shows that using polyimide capillaries leads to the overgrowth of supported Pt nanoparticles during reduction at temperatures below the glass transition temperature (Tg= 658 K) owing to an outgassing of water from the polyimide. Quartz capillaries were also studied and this overgrowth was not observed.

Structural and Chemical Characterization of Yb2O3-ZrO2 System by HAADF-STEM and HRTEM

2009 ◽  
Vol 15 (1) ◽  
pp. 46-53 ◽  
Author(s):  
C. Angeles-Chavez ◽  
P. Salas ◽  
L.A. Díaz-Torres ◽  
E. de la Rosa ◽  
R. Esparza ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Crystalline Structure ◽  
Sol Gel ◽  
Tetragonal Zirconia ◽  
Chemical Characterization ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractZrO2:Yb3+ nanocrystalline phosphors with high concentrations of ytterbium ions were prepared using the sol-gel method. X-ray diffraction, high-angle annular-dark-field scanning transmission electron microscopy (HAADF-STEM), energy dispersive X-ray spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to characterize the nanocrystalline phosphors annealed at 1000°C. Unit-cell distortion and changes in the crystalline structure of the monoclinic zirconia to tetragonal zirconia, and subsequently cubic zirconia, were observed with increased Yb concentration. Yb ions were randomly distributed into the lattice of the crystalline structure. No segregation of Yb2O3 phase was observed. The substitution of Zr atoms by Yb atoms on different crystalline phases was confirmed by the experimental results and theoretical simulations of HRTEM and HAADF-STEM.

scholarly journals Effects of Ag Additive in Low Temperature CO Detection with In2O3 Based Gas Sensors

Nanomaterials ◽  
2018 ◽  
Vol 8 (10) ◽  
pp. 801 ◽  
Author(s):  
Daniil Naberezhnyi ◽  
Marina Rumyantseva ◽  
Darya Filatova ◽  
Maria Batuk ◽  
Joke Hadermann ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Single Point ◽  
Active Surface ◽  
Dark Field ◽  
Hydroxyl Groups ◽  
X Ray ◽  
Surface Hydroxyl ◽  
Transmission Electron

Nanocomposites In2O3/Ag obtained by ultraviolet (UV) photoreduction and impregnation methods were studied as materials for CO sensors operating in the temperature range 25–250 °C. Nanocrystalline In2O3 and In2O3/Ag nanocomposites were characterized by X-ray diffraction (XRD), single-point Brunauer-Emmet-Teller (BET) method, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM) with energy dispersive X-ray (EDX) mapping. The active surface sites were investigated using Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), electron paramagnetic resonance (EPR) spectroscopy and thermo-programmed reduction with hydrogen (TPR-H2) method. Sensor measurements in the presence of 15 ppm CO demonstrated that UV treatment leads to a complete loss of In2O3 sensor sensitivity, while In2O3/Ag-UV nanocomposite synthesized by UV photoreduction demonstrates an increased sensor signal to CO at T < 200 °C. The observed high sensor response of the In2O3/Ag-UV nanocomposite at room temperature may be due to the realization of an additional mechanism of CO oxidation with participation of surface hydroxyl groups associated via hydrogen bonds.

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