Phase recovery and lensless imaging by iterative methods in optical, X-ray and electron diffraction

2002 ◽  
Vol 360 (1794) ◽  
pp. 875-895 ◽  
Author(s):  
J. C. H. Spence ◽  
U. Weierstall ◽  
M. Howells
Keyword(s):  
Electron Diffraction ◽  
Iterative Methods ◽  
Lensless Imaging ◽  
Phase Recovery ◽  
X Ray

Bimolecular and Monomolecular Lipid Films: Selected Area Electron Diffraction

1969 ◽  
Vol 27 ◽  
pp. 338-339
Author(s):  
Robert M. Glaeser ◽  
David W. Deamer
Keyword(s):  
Electron Diffraction ◽  
Membrane Structure ◽  
Molecular Organization ◽  
Membrane Material ◽  
X Ray Diffraction ◽  
Membrane Systems ◽  
X Ray ◽  
Selected Area Electron Diffraction ◽  
Lipid Films ◽  
Ultimate Objective

In the investigation of the molecular organization of cell membranes it is often supposed that lipid molecules are arranged in a bimolecular film. X-ray diffraction data obtained in a direction perpendicular to the plane of suitably layered membrane systems have generally been interpreted in accord with such a model of the membrane structure. The present studies were begun in order to determine whether selected area electron diffraction would provide a tool of sufficient sensitivity to permit investigation of the degree of intermolecular order within lipid films. The ultimate objective would then be to apply the method to single fragments of cell membrane material in order to obtain data complementary to the transverse data obtainable by x-ray diffraction.

Isomorphous replacement in electron diffraction of wet crystals of rat hemoglobin

1983 ◽  
Vol 41 ◽  
pp. 446-447
Author(s):  
William F. Tivol ◽  
Murray Vernon King ◽  
D. F. Parsons
Keyword(s):  
Electron Diffraction ◽  
Heavy Atom ◽  
Isomorphous Substitution ◽  
X Ray Diffraction ◽  
Salt Solutions ◽  
X Ray ◽  
Isomorphous Replacement ◽  
Structure Factors ◽  
Diffraction Structure ◽  
The Mean

Feasibility of isomorphous substitution in electron diffraction is supported by a calculation of the mean alteration of the electron-diffraction structure factors for hemoglobin crystals caused by substituting two mercury atoms per molecule, following Green, Ingram & Perutz, but with allowance for the proportionality of f to Z3/4 for electron diffraction. This yields a mean net change in F of 12.5%, as contrasted with 22.8% for x-ray diffraction.Use of the hydration chamber in electron diffraction opens prospects for examining many proteins that yield only very thin crystals not suitable for x-ray diffraction. Examination in the wet state avoids treatments that could cause translocation of the heavy-atom labels or distortion of the crystal. Combined with low-fluence techniques, it enables study of the protein in a state as close to native as possible.We have undertaken a study of crystals of rat hemoglobin by electron diffraction in the wet state. Rat hemoglobin offers a certain advantage for hydration-chamber work over other hemoglobins in that it can be crystallized from distilled water instead of salt solutions.

The structure of amorphous and polycrystalline materials using energy-filtered RDF analysis

1992 ◽  
Vol 50 (2) ◽  
pp. 1190-1191
Author(s):  
David Cockayne ◽  
David McKenzie
Keyword(s):  
Electron Diffraction ◽  
Diffraction Pattern ◽  
Density Function ◽  
Electron Diffraction Pattern ◽  
Polycrystalline Materials ◽  
Nearest Neighbour ◽  
X Ray ◽  
Selected Area Electron Diffraction ◽  
Reduced Density ◽  
System F

The technique of Electron Reduced Density Function (RDF) analysis has ben developed into a rapid analytical tool for the analysis of small volumes of amorphous or polycrystalline materials. The energy filtered electron diffraction pattern is collected to high scattering angles (currendy to s = 2 sinθ/λ = 6.5 Å-1) by scanning the selected area electron diffraction pattern across the entrance aperture to a GATAN parallel energy loss spectrometer. The diffraction pattern is then converted to a reduced density function, G(r), using mathematical procedures equivalent to those used in X-ray and neutron diffraction studies.Nearest neighbour distances accurate to 0.01 Å are obtained routinely, and bond distortions of molecules can be determined from the ratio of first to second nearest neighbour distances. The accuracy of coordination number determinations from polycrystalline monatomic materials (eg Pt) is high (5%). In amorphous systems (eg carbon, silicon) it is reasonable (10%), but in multi-element systems there are a number of problems to be overcome; to reduce the diffraction pattern to G(r), the approximation must be made that for all elements i,j in the system, fj(s) = Kji fi,(s) where Kji is independent of s.

Evidence for ordered Fe3Ni

1987 ◽  
Vol 45 ◽  
pp. 216-217
Author(s):  
K.B. Reuter ◽  
D.B. Williams ◽  
J.I. Goldstein
Keyword(s):  
Experimental Data ◽  
Martensitic Transformation ◽  
Electron Diffraction ◽  
Room Temperature ◽  
Direct Evidence ◽  
Transformation Product ◽  
Iron Meteorites ◽  
X Ray ◽  
Ni Content ◽  
Temperature Transformation

In the Fe-Ni system, although ordered FeNi and ordered Ni3Fe are experimentally well established, direct evidence for ordered Fe3Ni is unconvincing. Little experimental data for Fe3Ni exists because diffusion is sluggish at temperatures below 400°C and because alloys containing less than 29 wt% Ni undergo a martensitic transformation at room temperature. Fe-Ni phases in iron meteorites were examined in this study because iron meteorites have cooled at slow rates of about 10°C/106 years, allowing phase transformations below 400°C to occur. One low temperature transformation product, called clear taenite 2 (CT2), was of particular interest because it contains less than 30 wtZ Ni and is not martensitic. Because CT2 is only a few microns in size, the structure and Ni content were determined through electron diffraction and x-ray microanalysis. A Philips EM400T operated at 120 kV, equipped with a Tracor Northern 2000 multichannel analyzer, was used.

Electron diffraction studies of amorphous and polycrystalline thin films

1990 ◽  
Vol 48 (4) ◽  
pp. 118-119
Author(s):  
D J H Cockayne ◽  
D R McKenzie
Keyword(s):  
Thin Films ◽  
Electron Diffraction ◽  
Polycrystalline Materials ◽  
Good Resolution ◽  
Scattered Intensity ◽  
Radial Density ◽  
X Ray ◽  
Polycrystalline Thin Films ◽  
Nitrogen Ion ◽  
Diffraction Patterns

The study of amorphous and polycrystalline materials by obtaining radial density functions G(r) from X-ray or neutron diffraction patterns is a well-developed technique. We have developed a method for carrying out the same technique using electron diffraction in a standard TEM. It has the advantage that studies can be made of thin films, and on regions of specimen too small for X-ray and neutron studies. As well, it can be used to obtain nearest neighbour distances and coordination numbers from the same region of specimen from which HREM, EDS and EELS data is obtained.The reduction of the scattered intensity I(s) (s = 2sinθ/λ ) to the radial density function, G(r), assumes single and elastic scattering. For good resolution in r, data must be collected to high s. Previous work in this field includes pioneering experiments by Grigson and by Graczyk and Moss. In our work, the electron diffraction pattern from an amorphous or polycrystalline thin film is scanned across the entrance aperture to a PEELS fitted to a conventional TEM, using a ramp applied to the post specimen scan coils. The elastically scattered intensity I(s) is obtained by selecting the elastically scattered electrons with the PEELS, and collecting directly into the MCA. Figure 1 shows examples of I(s) collected from two thin ZrN films, one polycrystalline and one amorphous, prepared by evaporation while under nitrogen ion bombardment.

Microstructure and crystal symmetry of Pb2Sr2(Y/Ca)Cu3O9−δ

1990 ◽  
Vol 48 (4) ◽  
pp. 64-65
Author(s):  
Y. P. Lin ◽  
J. S. Xue ◽  
J. E. Greedan
Keyword(s):  
Electron Diffraction ◽  
High Temperature Superconductors ◽  
Carbon Film ◽  
Basic Structure ◽  
Crystal Symmetry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Space Groups ◽  
New Family ◽  
Convergent Beam

A new family of high temperature superconductors based on Pb2Sr2YCu3O9−δ has recently been reported. One method of improving Tc has been to replace Y partially with Ca. Although the basic structure of this type of superconductors is known, the detailed structure is still unclear, and various space groups has been proposed. In our work, crystals of Pb2Sr2YCu3O9−δ with dimensions up to 1 × 1 × 0.25.mm and with Tc of 84 K have been grown and their superconducting properties described. The defects and crystal symmetry have been investigated using electron microscopy performed on crushed crystals supported on a holey carbon film.Electron diffraction confirmed x-ray diffraction results which showed that the crystals are primitive orthorhombic with a=0.5383, b=0.5423 and c=1.5765 nm. Convergent Beam Electron Diffraction (CBED) patterns for the and axes are shown in Figs. 1 and 2 respectively.

Microdomains in BaFeO3-y (0.35 < y < 0.50)

1990 ◽  
Vol 48 (4) ◽  
pp. 780-781
Author(s):  
M. Vallet-Regí ◽  
M. Parras ◽  
J.M. González-Calbet ◽  
J.C. Grenier
Keyword(s):  
Electron Diffraction ◽  
Chemical Analysis ◽  
Monoclinic Phase ◽  
Orthorhombic Phase ◽  
Total Iron ◽  
Zone Axis ◽  
Electron Micrograph ◽  
X Ray Diffraction ◽  
X Ray ◽  
Compositional Variations

BaFeO3-y compositions (0.35<y<0.50) have been investigated by means of electron diffraction and microscopy to resolve contradictory results from powder X-ray diffraction data.The samples were obtained by annealing BaFeO2.56 for 48 h. in the temperature range from 980°C to 1050°C . Total iron and barium in the samples were determined using chemical analysis and gravimetric methods, respectively.In the BaFeO3-y system, according to the electron diffraction and microscopy results, the nonstoichiometry is accommodated in different ways as a function of the composition (y):In the domain between BaFeO2.5+δBaFeO2.54, compositional variations are accommodated through the formation of microdomains. Fig. la shows the ED pattern of the BaFeO2.52 material along thezone axis. The corresponding electron micrograph is seen in Fig. 1b. Several domains corresponding to the monoclinic BaFeO2.50 phase, intergrow with domains of the orthorhombic phase. According to that, the ED pattern of Fig. 1a, can be interpreted as formed by the superposition of three types of diffraction maxima : Very strong spots corresponding to a cubic perovskite, a set of maxima due to the superposition of three domains of the monoclinic phase along [100]m and a series of maxima corresponding to three domains corresponding to the orthorhombic phase along the [100]o.

An Electron Diffraction Study on Litnerized Potato Starch

1990 ◽  
Vol 48 (1) ◽  
pp. 580-581
Author(s):  
Jean-Claude Jésior ◽  
Roger Vuong ◽  
Henri Chanzy
Keyword(s):  
Electron Microscope ◽  
Electron Diffraction ◽  
Signal To Noise Ratio ◽  
Potato Starch ◽  
Image Intensifier ◽  
Electron Diffraction Study ◽  
Starch Granules ◽  
X Ray ◽  
Individual Grains ◽  
Diamond Knife

Starch is arranged in a crystalline manner within its storage granules and should thus give sharp X-ray diagrams. Unfortunately most of the common starch granules have sizes between 1 and 100μm, making them too small for an X-ray study on individual grains. There is only one instance where an oriented X-ray diagram could be obtained on one sector of an individual giant starch granule. Despite their small size, starch granules are still too thick to be studied by electron diffraction with a transmission electron microscope. The only reported study on starch ultrastructure using electron diffraction on frozen hydrated material was made on small fragments. The present study has been realized on thin sectioned granules previously litnerized to improve the signal to noise ratio.Potato starch was hydrolyzed for 10 days in 2.2N HCl at 35°C, dialyzed against water until neutrality and embedded in Nanoplast. Sectioning was achieved with a commercially available low-angle “35°” diamond knife (Diatome) after a very carefull trimming and a pre-sectioning with a classical “45°” diamond knife. Sections obtained at a final sectioning angle of 42.2° (compared with the usual 55-60°) and at a nominal thickness of 900Å were collected on a Formvar-carbon coated grid. The exact location of the starch granules in their sections was recorded by optical microscopy on a Zeiss Universal polarizing microscope (Fig. 1a). After rehydration at a relative humidity of 95% for 24 hours they were mounted on a Philips cryoholder and quench frozen in liquid nitrogen before being inserted under frozen conditions in a Philips EM 400T electron microscope equipped with a Gatan anticontaminator and a Lhesa image intensifier.

Electron diffraction detection of ordliking in annealed PbTe thin film

1990 ◽  
Vol 48 (4) ◽  
pp. 1018-1019
Author(s):  
Karimat El-Sayed
Keyword(s):  
Thin Film ◽  
Electron Diffraction ◽  
Lead Telluride ◽  
Structural Basis ◽  
Face Centered Cubic ◽  
X Ray ◽  
Polycrystalline Thin Films ◽  
Stage Process ◽  
Diffraction Patterns ◽  
Face Centered

Lead telluride is an important semiconductor of many applications. Many Investigators showed that there are anamolous descripancies in most of the electrophysical properties of PbTe polycrystalline thin films on annealing. X-Ray and electron diffraction studies are being undertaken in the present work in order to explain the cause of this anamolous behaviour.Figures 1-3 show the electron diffraction of the unheated, heated in air at 100°C and heated in air at 250°C respectively of a 300°A polycrystalline PbTe thin film. It can be seen that Fig. 1 is a typical [100] projection of a face centered cubic with unmixed (hkl) indices. Fig. 2 shows the appearance of faint superlattice reflections having mixed (hkl) indices. Fig. 3 shows the disappearance of thf superlattice reflections and the appearance of polycrystalline PbO phase superimposed on the [l00] PbTe diffraction patterns. The mechanism of this three stage process can be explained on structural basis as follows :

Dynamical Scattering in Electron Diffraction of wet Protein Crystals

1980 ◽  
Vol 38 ◽  
pp. 42-43
Author(s):  
B. B. Chang ◽  
D. F. Parsons
Keyword(s):  
Electron Diffraction ◽  
Scattering Theory ◽  
Protein Crystals ◽  
Electron Diffraction Data ◽  
Specimen Thickness ◽  
Major Question ◽  
X Ray ◽  
Scattering Effects ◽  
Diffraction Patterns ◽  
Acceleration Voltage

The significance of dynamical scattering effects remains the major question in the structural analysis by electron diffraction of protein crystals preserved in the hydrated state. In the few cases (single layers of purple membrane and 400-600 Å thick catalase crystals examined at 100 kV acceleration voltage) where electron-diffraction patterns were used quantitatively, dynamical scattering effects were considered unimportant on the basis of a comparison with x-ray intensities. The kinematical treatment is usually justified by the thinness of the crystal. A theoretical investigation by Ho et al. using Cowley-Moodie multislice formulation of dynamical scattering theory and cytochrome b5as the test object2 suggests that kinematical analysis of electron diffraction data with 100-keV electrons would not likely be valid for specimen thickness of 300 Å or more. We have chosen to work with electron diffraction patterns obtained from actual wet protein crystals (rat hemoglobin crystals of thickness range 1000 to 2500 Å) at 200 and 1000 kV and to analyze these for dynamical effects.

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