scholarly journals MicroED: a versatile cryoEM method for structure determination

2018 ◽  
Vol 2 (1) ◽  
pp. 1-8 ◽  
Author(s):  
Brent L. Nannenga ◽  
Tamir Gonen
Keyword(s):  
Electron Microscope ◽  
High Resolution ◽  
Electron Diffraction ◽  
Structure Determination ◽  
Materials Science ◽  
Electron Diffraction Data ◽  
Determination Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron

Micro-electron diffraction, or MicroED, is a structure determination method that uses a cryo-transmission electron microscope to collect electron diffraction data from nanocrystals. This technique has been successfully used to determine the high-resolution structures of many targets from crystals orders of magnitude smaller than what is needed for X-ray diffraction experiments. In this review, we will describe the MicroED method and recent structures that have been determined. Additionally, applications of electron diffraction to the fields of small molecule crystallography and materials science will be discussed.

Synthesis of one-dimensional structured metal phthalocyanine in an ionic liquid

2007 ◽  
Vol 11 (10) ◽  
pp. 713-718 ◽  
Author(s):  
David S. Jacob ◽  
Somashekarappa Mallenahalli ◽  
Aharon Gedanken ◽  
Leonid A. Solovyov ◽  
Evangelia Xenogiannopoulou ◽  
...  
Keyword(s):  
Ionic Liquid ◽  
Electron Microscope ◽  
High Resolution ◽  
High Yield ◽  
Metal Phthalocyanine ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Nickel Phthalocyanine ◽  
Transmission Electron

Nickel phthalocyanine is synthesized in an ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate) giving a high yield of one-dimensional structures. The morphology of the synthesized material is detected by a high-resolution scanning electron microscope, a high-resolution transmission electron microscope, characterized by powder X-ray diffraction, and a CHN analyzer. The nonlinear optical properties of the synthesized phthalocyanine are also investigated.

HRTEM Observation of Rod-Shape Precipitates in Al-Mg-Si-Ag Alloy Aged at 523 K

2007 ◽  
Vol 561-565 ◽  
pp. 243-246 ◽  
Author(s):  
Junya Nakamura ◽  
Kenji Matsuda ◽  
Yoshio Nakamura ◽  
Tatsuo Sato ◽  
Susumu Ikeno
Keyword(s):  
Crystal Structure ◽  
Electron Microscope ◽  
High Resolution ◽  
Electron Diffraction ◽  
Metastable Phase ◽  
X Ray ◽  
Β Phase ◽  
Selected Area Electron Diffraction ◽  
Transmission Electron ◽  
Hrtem Observation

The purpose of this study is to identify the crystal structure of metastable phase in Ag added Al-Mg-Si alloy to compare the formation of β’-phases in Al-Mg-Si alloys without Ag, using images of high resolution transmission electron microscope (HRTEM), selected area electron diffraction (SAED) patterns and an energy dispersive X-ray spectroscopy (EDS). The result of SAED patterns and HRTEM images have been simulated and compared with images then SAED patterns obtained from actual precipitates. SAED patterns and HRTEM images obtained from metastable phase in the Ag added Al-Mg-Si alloy showed similar to those of β’-phase in Al-Mg-Si alloy without Ag and the lattice spacings changed because of the effect of Ag.

Electron beam-induced surface modification and nano-engineering of carbon nanotubes: Single-walled and multiwalled

2006 ◽  
Vol 21 (12) ◽  
pp. 3109-3123 ◽  
Author(s):  
S. Gupta ◽  
R.J. Patel ◽  
R.E. Giedd
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Raman Spectroscopy ◽  
Electron Beam ◽  
Electron Microscope ◽  
High Resolution ◽  
Band Intensity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron

Influence of low and medium energy electron beam (E-beam) irradiation on the single-walled (SW) and multiwalled (MW) carbon nanotube films grown by microwave chemical vapor deposition are investigated. These films were subjected to electron beam energy of 50 keV from scanning electron microscope for 2.5, 5.5, 8.0, and 15 h and 100, 200, and 300 keV from transmission electron microscope electron gun for a few minutes to approximately 2 h continuously. To assess the surface modifications/structural degradation, the films were analyzed prior to and post-irradiation using x-ray diffraction and micro-Raman spectroscopy in addition to in situ monitoring by scanning and high-resolution transmission electron microscopy. A minimal increase in intertube or interplanar spacing (i.e., d002) for MW nanotubes ranging from 3.25–3.29 Å (∼3%) can be analogized to change in c-axis of graphite lattice due to thermal effects measured using x-ray diffraction. Resonance Raman spectroscopy revealed that irradiation generated defects in the lattice evaluated through variation of: the intensity of radial breathing mode (RBM), intensity ratio of D to G band (ID/IG), position of D and G bands and their harmonics (D* and G*). The increase in the defect-induced D band intensity, quenching of RBM intensity, and only a slight increase in G band intensity are some of the implications. The MW nanotubes tend to reach a state of saturation for prolonged exposures, while SW transforming semiconducting to quasi-metallic character. Softening of the q = 0 selection rule is suggested as a possible way to explain these results. It is also suggestive that knock-on collision may not be the primary cause of structural degradation, rather a local gradual reorganization, i.e., sp2+δ ⇔ sp2+δ, sp2 C seems quite possible. Experiments showed that with extended exposures, both kinds of nanotubes displayed various local structural instabilities including pinching, graphitization/amorphization, and forming intra-molecular junction (IMJ) within the area of electron beam focus possibly through amorphous carbon aggregates. They also displayed curling and closure forming nano-ring and helix-like structures while mending their dangling bonds. High-resolution transmission electron microscopy electrons corroborated these conclusions. Manufacturing of nanoscale structures “nano-engineering” of carbon-based systems is tentatively ascribed to irradiation-induced solid-state phase transformation, in contrast to conventional nanotube synthesis from the gas phase.

Complex Superstructures Resulting from Compositional Modulation and Octahedral Tilt Twinning in AA′BB′O6 Doubly Cation Ordered Perovskites

2013 ◽  
Vol 2013 (CICMT) ◽  
pp. 000006-000013
Author(s):  
Graham King ◽  
Susana Garcia-Martin ◽  
Esteban Urones-Garrote ◽  
Gwilherm Nenert ◽  
Patrick M. Woodward
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Resolution ◽  
Electron Diffraction ◽  
Neutron Powder Diffraction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Compositional Modulation ◽  
System A ◽  
Transmission Electron

The ordering of cations within the perovskite structure can have a profound effect on the physical properties. A number of AA′BB′O6 perovskite phases which have both a rock salt ordering of the B/B′ cations and a layered ordering of the A/A′ cations have recently been prepared and studied. In some of these compositions complex nanoscale superstructure formation has been observed. These superstructures are the result of compositional modulations involving the occupancies of the A and A′ cations and are accompanied by a twinning of the octahedral tilt system. A wide variety of patterns are observed, such as 1-dimensional stripes or 2-dimensional chessboards which can have periodicities which are either commensurate or incommensurate with the underlying subcell. These superstructures cannot be easily detected by powder X-ray diffraction but have been observed using a combination of high resolution transmission electron microscopy, electron diffraction, and neutron powder diffraction. The factors which determine the dimensionality and periodicity of the superstructures are discussed and compared with the closely related Li based perovskite systems.

Synthesis of Hollow Carbon Hemispheres in the Magnesium Carbonate-Metallic Li System with the Help of CHBr3

2011 ◽  
Vol 266 ◽  
pp. 106-109
Author(s):  
Jia Fu Chen ◽  
Zhi Min Chen ◽  
Yan Cao ◽  
Qun Xu
Keyword(s):  
Electron Microscope ◽  
Electron Diffraction ◽  
Single Layer ◽  
Magnesium Carbonate ◽  
X Ray Diffraction ◽  
Graphite Phase ◽  
X Ray ◽  
Transmission Electron ◽  
Hollow Carbon ◽  
Scanning Electron

Hollow carbon hemispheres (HCHs) were synthesized at 500 oC in the magnesium carbonate-metallic Li system with the help of CHBr3. The product was characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and field emission scanning electron microscope (FESEM). XRD and electron diffraction (ED) pattern results showed that HCHs were graphite phase and polycrystalline. By FESEM and TEM observation, the diameters of the HCHs were in the range of 200-900 nm. The shell of the HCHs was single-layer and their thickness was about 31 nm. The formation mechanism of HCHs with the help of CHBr3 was discussed. Besides, the effect of reaction temperature and dosage of CHBr3 on the morphology of HCHs was studied.

scholarly journals Resolution of a modulated structure by electron and powder X-ray diffraction

2014 ◽  
Vol 70 (a1) ◽  
pp. C928-C928
Author(s):  
Christophe Lepoittevin ◽  
Olivier Leynaud
Keyword(s):  
Electron Diffraction ◽  
Structure Determination ◽  
Structural Model ◽  
Zone Axis ◽  
Reciprocal Space ◽  
Electron Diffraction Data ◽  
X Ray Diffraction ◽  
Precession Angle ◽  
X Ray ◽  
Cell Parameters

These past few years, many new structures have been solved using electron diffraction methods: zone axis precession electron diffraction (PED) and tomography in reciprocal space. Both methods enable to reduce importantly the multiple scattering, so that the reflection intensities can be used for structure determination by direct methods. The ferrite Sr25Fe30O77 belongs to a family of phases whose structures consist of an intergrowth of m perovskite layers with complex rocksalt type layers [1,2]. The compound of interest is the member m = 4 of this family and its structure has been solved by combining both electron diffraction methods cited above. This oxide crystallizes in an orthorhombic system with the sub-cell parameters a ≍ b ≍ 5.4 Å and c ≍ 42 Å in a F type lattice. The structure exhibits modulation along a axis with a modulation vector q = 2/5 a. The commensurate nature of the modulation enables to describe the structure in a supercell with the cell parameters a ≍ 27 Å, b ≍ 5.4 Å and c ≍ 42 Å. PED patterns were recorded in zone axis with a Spinning Star unit using a precession angle of 20. The intensities were extracted with CRISP software and the resulting dataset was then implemented in SIR2008 for structure solution. The tomography data collection, recorded by tilting manually every 0.5 degree from -30 to +30 degrees, was inserted in a "3D Electron Diffraction Tomography" software, which reconstructs the 3D reciprocal space and extracts automatically the reflection intensities. The intensity file was then used on SIR2008 for structure determination. In order to confirm and refine the structural model, a powder X-ray diffraction pattern was performed on a laboratory diffractometer with Cu Ka1 radiation. Cell parameters were refined with the WinPlotr and FullProf Softwares using both LeBail and Rietveld methods [3]. The structural model obtained with electron diffraction data was tried and confirmed as the correct structure by the Rietveld refinements.

Nano-Structural Alteration of Pyrophyllite by Grinding Revealed by X-Ray Diffraction and High-Resolution Transmission Electron Microscopy

2016 ◽  
Vol 40 ◽  
pp. 72-78 ◽  
Author(s):  
Jia Wei Sheng ◽  
Li Ping Zhang ◽  
Jun Yan ◽  
Qing Sun ◽  
Jian Zhang
Keyword(s):  
Electron Microscope ◽  
High Resolution ◽  
Ball Mill ◽  
Structural Alteration ◽  
X Ray Diffraction ◽  
Mechanical Destruction ◽  
X Ray ◽  
Selected Area Electron Diffraction ◽  
Transmission Electron ◽  
Scanning Electron

The mechanical destruction of the pyrophyllite structure and final ground products upon grinding with a laboratory planetary ball mill were investigated using high-resolution transmission electron microscope (HRTEM) coupled with selected area electron diffraction (SAED), field emission scanning electron microscope (SEM) and X-ray diffraction (XRD). Grinding produced a profound structural alteration, resulting in increasing amorphization. Increasing the intensity of grinding resulted in acceleration of the mechanically induced amorphization of the pyrophyllite structure. The pyrophyllite phase was transformed into its anhydride phase during the process of the prolonged grinding. Increasing the grinding intensity resulted in faster destruction of the pyrophyllite structure. The plate-like microcrystal exhibited the 2M-pyrophyllite crystal structure. The pyrophyllite anhydride phase was existed after grinding.

scholarly journals Refinements on electron diffraction data of β-glycine in MoPro: a quest for an improved structure model

2021 ◽  
Vol 54 (4) ◽  
Author(s):  
Kunal Kumar Jha ◽  
Barbara Gruza ◽  
Michał Leszek Chodkiewicz ◽  
Christian Jelsch ◽  
Paulina Maria Dominiak
Keyword(s):  
Electron Diffraction ◽  
Diffraction Data ◽  
Structure Determination ◽  
Structure Refinement ◽  
Electron Diffraction Data ◽  
Bethe Equation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Atom Model ◽  
X Ray Scattering

The advancement in 3D electron diffraction (3D ED) techniques that lead to a revolution in molecular structure determination using nano-sized crystals is now achieving atomic resolution. The structures can be obtained from 3D ED data with tools similar to those used for X-ray structure determination. In this context, the MoPro software, originally designed for structure and charge density refinements using X-ray diffraction data, has been adapted. Structure refinement on 3D ED data was achieved via implementation of electron scattering factors available in the literature and by application of the Mott–Bethe equation to X-ray scattering factors computed from the multipolar atom model. The multipolar model was parametrized using the transferable pseudoatom databanks ELMAM2 and UBDB. Applying the independent atom model (IAM), i.e. spherical neutral atom refinement, to 3D ED data on β-glycine in MoPro resulted in structure and refinement statistics comparable to those obtained from other well known software. Use of the transferred aspherical atom model (TAAM) led to improvement of the refinement statistics and a better fit of the model to the 3D ED data as compared with the spherical atom refinement. The anisotropic displacement parameters of non-H atoms appear underestimated by typically 0.003 Å2 for the non-H atoms in IAM refinement compared with TAAM. Thus, MoPro is shown to be an effective tool for crystal structure refinement on 3D ED data and allows use of a spherical or a multipolar atom model. Electron density databases can be readily transferred with no further modification needed when the Mott–Bethe equation is applied.

A High Resolution Study of G.P. Zones in Aluminum - 4.2 at % Silver

1982 ◽  
Vol 40 ◽  
pp. 722-723 ◽  
Author(s):  
R. Gronsky
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Resolution ◽  
Computer Simulations ◽  
Structural Characteristics ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Resolution Study

The phenomenon of clustering in Al-Ag alloys has been extensively studied since the early work of Guinierl, wherein the pre-precipitation state was characterized as an assembly of spherical, ordered, silver-rich G.P. zones. Subsequent x-ray and TEM investigations yielded results in general agreement with this model. However, serious discrepancies were later revealed by the detailed x-ray diffraction - based computer simulations of Gragg and Cohen, i.e., the silver-rich clusters were instead octahedral in shape and fully disordered, atleast below 170°C. The object of the present investigation is to examine directly the structural characteristics of G.P. zones in Al-Ag by high resolution transmission electron microscopy.

Luminescent Properties of Gd2MoO6:Eu3+ Nanophosphor for WLEDs

2021 ◽  
Author(s):  
Yan Chen ◽  
Yuemei Lan ◽  
Dong Wang ◽  
Guoxing Zhang ◽  
Wenlong Peng ◽  
...  
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Fluorescence Spectra ◽  
Solvothermal Method ◽  
Luminescent Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron

A series of Gd2-xMoO6:xEu3+(x=0.18-0.38) nanophosphors were synthesized by the solvothermal method. The properties of this nanophosphor were characterized by x-ray diffraction (XRD), transmission electron microscope (TEM), fluorescence spectra and diffuse...

Sign in / Sign up

Export Citation Format

Share Document