Search results for "Electron diffraction"
showing 10 items of 191 documents
ChemInform Abstract: Solution Synthesis of a New Thermoelectric Zn1+xSb Nanophase and Its Structure Determination Using Automated Electron Diffractio…
2010
Thermoelectric nanoparticles of the nominal composition Zn4Sb3 are prepared by heating Sb nanoparticles with a 9-fold excess of Zn particles (synthesized by reaction of SbCl3 or ZnCl2 with Li[Et3BH] in THF at room temperature, and about 65 °C, respectively) in trioctylamine at about 300 °C for 225 min.
Microphase separation upon crystallization of small amphiphilic molecules: ‘low’ temperature form II of sodium benzoate (E 211)
2016
A so far unknown low temperature polymorph (form II crystallized at 350 °C) of the common food preservative sodium benzoate (NaBz; E 211) could be crystallized by annealing (7 days) of the poorly crystalline technical material. Its crystal structure was solved by indexing a tiny single crystal by electron diffraction followed by structure solution and refinement applying powder X-ray diffraction (PXRD). The new polymorph shows many structural similarities to form I (crystallized at 420 °C). Both form I and II are the result of a microphase separation: the structures consist of pseudo-hexagonal packings of rod-shaped micelles where the core consists of sodium cations being coordinated by the…
Heteroeptiaxial growth of alloy monolayers on W(110)
2005
Abstract We studied the initial growth of Co 1 - x Fe x films on W(1 1 0) using scanning tunneling microscopy and spectroscopy (STM and STS), in combination with low-energy electron diffraction (LEED). For Co-rich alloys the deposition at room temperature followed by high-temperature annealing is not equivalent to the deposition at high substrate temperatures, in contrast to the case of Fe-rich alloys. While room temperature deposition results in a structure consisting of small islands even after annealing, deposition at high substrate temperatures leads to large coalesced areas. Sequential deposition of pure Co and pure Fe results in phase separated areas of Co- and Fe-rich areas. Only, in…
Reactivity between molybdenum and TiO2(110) surfaces: evidence of a sub-monolayer mode and a multilayer mode
2005
Small amounts of molybdenum (from 0.03 to 1.3 eqML) were deposited on non-stoichiometric TiO 2 (1 1 0) surface. The deposits were investigated by means of LEED and X-ray/UV photoemission using synchrotron radiation. For the smallest coverage (<0.2 eqML), deposition leads to oxidation of molybdenum into species close to Mo 4+ .In such a case, states appearing in TiO 2 band gap are mainly due to reduced titanium. For higher coverages, metallic behaviour of molybdenum is observed. This phenomenon was explained, thanks to first principle calculations, as a decrease of the Mo-O interactions for the benefit of the Mo-Mo interactions as the surface molybdenum atom density increases.
Solution Synthesis of a New Thermoelectric Zn1-xSb Nanophase and Its Structure Determination Using Automated Electron Diffraction Tomography
2010
Engineering materials with specific physical properties have recently focused on the effect of nanoscopic inhomogeneities at the 10 nm scale. Such features are expected to scatter medium- and long-wavelength phonons thereby lowering the thermal conductivity of the system. Low thermal conductivity is a prerequisite for effective thermoelectric materials, and the challenge is to limit the transport of heat by phonons, without simultaneously decreasing charge transport. A solution-phase technique was devised for synthesis of thermoelectric "Zn(4)Sb(3)" nanocrystals as a precursor for phase segregation into ZnSb and a new Zn-Sb intermetallic phase, Zn(1+delta)Sb, in a peritectoid reaction. Our …
Atomic structure solution of the complex quasicrystal approximant Al77Rh15Ru8 from electron diffraction data
2014
The crystal structure of the novel Al77Rh15Ru8phase (which is an approximant of decagonal quasicrystals) was determined using modern direct methods (MDM) applied to automated electron diffraction tomography (ADT) data. The Al77Rh15Ru8E-phase is orthorhombic [Pbma,a= 23.40 (5),b= 16.20 (4) andc= 20.00 (5) Å] and has one of the most complicated intermetallic structures solved solely by electron diffraction methods. Its structural model consists of 78 unique atomic positions in the unit cell (19 Rh/Ru and 59 Al). Precession electron diffraction (PED) patterns and high-resolution electron microscopy (HRTEM) images were used for the validation of the proposed atomic model. The structure of the E…
Anion ordering and defect structure in Ruddlesden-Popper strontium niobium oxynitrides
2004
The crystal structure of the n = 1 member of the Ruddlesden-Popper family (SrO)(SrNbO(2)N)(n) was refined by the Rietveld method using neutron powder diffraction data. This complex crystallizes in the I4/mmm space group with cell parameters a = 4.0506(2) and c = 12.5936(9) angstroms. The refined composition was Sr(2)NbO(3.28)N(0.72), which corresponds to a formal oxidation state for Nb of +4.72, meaning 72% Nb(V) and 28% Nb(IV). The nitrogen atoms order in the equatorial sites of the niobium octahedra according to Pauling's second crystal rule as the more charged anion occupies the site showing the larger bond strength sums. Pauling's second crystal rule is shown to be able to predict the d…
Structure, energy and charge transport in two-dimensional crystals of cyanine dyes
1993
Abstract In order to develop systems with controlled energy or charge transfer across molecular dimensions it is highly desirable to build two-dimensional crystals of functional dye molecules: they can be addressed from the third dimension and the lateral intermolecular interactions can be well characterized due to a fixed and defined geometry. In an effort to study these possibilities we prepared crystals of different, negatively charged cyanine dyes, formed after adsorption from a water subphase to a positively charged monolayer. These crystals are one monolayer thick, of uniform dimensions between 10 and 100 μm (depending on nucleation conditions) and of rectangular shape. Single crystal…
Relationships between fatty acid monolayer structure on the subphase and on solid substrates
1991
Abstract Docosanoic acid monolayers with known molecular packings on the water surface have been deposited on thin polymer films and then investigated using transmission electron diffraction at normal and tilted incidence. The diffraction patterns from monolayers deposited under all conditions investigated could be indexed as arising from the same conformationally disordered centred rectangular packing with molecules standing perpendicular to the substrate, although with a spread of unit cell parameters within and between each deposition condition significantly greater than the experimental error. This packing has been seen in monolayers on the water surface, but only under conditions compl…
Comparison of electron diffraction data from non-linear optically active organic DMABC crystals obtained at 100 and 300 kV
2000
During the recent past, we have synthesized a new class of molecules with intramolecular two-dimensional charge transfer upon excitation. The present report presents such a molecule, 2,6-bis(4-dimethylamino-benzylidene)-cyclohexanone (DMABC), with an unusually high value of the second-order non-linear optical (NLO) coefficients. In order to optimize the macroscopic NLO properties of the compounds, it is necessary to relate their first hyperpolarizability tensors at a molecular level to those at a crystal bulk level. This requires a complete structure determination and refinement. However, the growth of sufficiently large single crystals, which are needed for structural analysis and refineme…