Corrosion inhibitor by a polymerizable columnar mesogen based on hexabenzocoronene derivative

A hexa-peri-hexabenzocoronene derivative (HBC-1,2,4-Ph-DA-C₁₂) with the central HBC core tethered with three diacetylene (DA)-containing chains and three saturated alkyl chains was applied for the anticorrosion of an iron surface. This compound, which exhibits a columnar liquid crystalline phase, could be polymerized by ultraviolet irradiation through reactions between the DA units. This polymer coating exhibited a good anticorrosion property with good hydrophobicity (contact angle [CA] ~ 84°–105°) and excellent mechanical property. It showed a high resistance of 149 kΩ/cm², much higher than that of known anticorrosion materials.     

Studies of the alignment properties of antiferroelectric liquid crystals by X-ray diffraction

It is observed optically that in a parallel rubbed antiferroelectric liquid crystal device, the texture consists of domains with two distinct optic axes, which make equal and opposite angles with the rubbing direction. It is proposed that this is caused by a large electroclinic effect at the surfaces during layer formation in the SmA* phase. This hypothesis is verified by finding the layer structure in single, parallel and skew rubbed devices by using X-ray diffraction.     

Phase transition sequence in ferroelectric Aurivillius compounds investigated by single crystal X-ray diffraction

The investigation of the phase transition sequence in SrBi₂Ta₂O₉ (SBT) and SrBi₂Nb₂O₉ (SBN) is reported using single-crystal X-ray diffraction. By monitoring specific reflections as a function of temperature, sensitive either to the superstructure formation or to polar displacements, it was possible to check the existence or not of an intermediate phase. This latter was confirmed in SBT, but within experimental accuracy could not be detected in SBN.     

The binding and correlation effects in carbon dioxide as investigated by gas X-ray diffraction

The X-ray scattering intensities of gaseous carbon dioxide have been measured by the enerey-dispersive method. Comparison of the measured intensities with theoretical calculations by the Hartree-Fock independent-atom model revealed the binding effect in the small-s region, which is largely consistent with theoretical predictions based on the molecular Hartree-Fock wavefunction.     

Effect of interfaces on the alignment of a discotic liquid-crystalline phthalocyanine

This paper deals with the influence of the nature and number of solid interfaces on the alignment of the columns in a semiconducting discotic liquid crystal. The solid substrates have been characterized in terms of their roughness and surface energy. The alignment of the discotic liquid crystal columns on these substrates has been determined by optical microscopy under crossed polarizers and by tapping-mode atomic force microscopy. The nature of the substrates has negligible influence on the alignment. The key parameter is the confinement imposed to the film. These surprising observations are explained by the antagonist alignment role of gas and solid interfaces.     

Ultrafast spin-state photoswitching in a crystal and slower consecutive processes investigated by femtosecond optical spectroscopy and picosecond X-ray diffraction

We report the spin state photo-switching dynamics in two polymorphs of a spin-crossover molecular complex triggered by a femtosecond laser flash, as determined by combining femtosecond optical pump-probe spectroscopy and picosecond X-ray diffraction techniques. The light-driven transformations in the two polymorphs are compared. Combining both techniques and tracking how the X-ray data correlate with optical signals allow understanding of how electronic and structural degrees of freedom couple and play their role when the switchable molecules interact in the active crystalline medium. The study sheds light on crossing the border between femtochemistry at the molecular scale and femtoswitching at the material scale.     

New insights on structural dynamics of electrochemical interface by time-resolved surface X-ray diffraction

Many time-resolved measurements of electrochemical interface have been developed in conformity with the time scale of various transition. X-ray diffraction using synchrotron radiation is a powerful tool for structural determination of electrical double layer in real time. This short review describes structural dynamics of interfacial ions during the faraday and non-faraday processes in the time scale from microsecond to second.     

Single crystal X-ray diffraction study of 2,4,6-triazidopyridine and its 3,5-dibromosubstituted derivative

By the single crystal X-ray diffraction analysis in combination with quantum chemical calculations the molecular and crystal structures of high-energy 2,4,6-triazidopyridine and 2,4,6-triazido-3,5- dibromopyridine are studied; the dependence of structural parameters of their azido groups on the size of substituents in β-positions of the pyridine ring is analyzed. The effect of the intramolecular contact involving the central nitrogen atom of γ-azido groups in substituted triazides on their structure and properties is revealed.     

Grazing incidence X-ray diffraction analysis of surface modified SiC layers

Thin films of silicon carbide with codeposited elemental silicon were prepared by chemical vapor deposition (CVD). In a second CVD-process a thin titanium layer was deposited on the SiC(Si) basic layer. The solid state reaction between titanium and the codeposited silicon can be observed by X-ray diffractometry. A helpful analytical method for the observation of the growth of the reaction products is grazing incidence X-ray diffractometry. Various diffraction patterns of titanium silicides can be obtained by decreasing incidence angles. Received: 24 June 1996 / Accepted: 5 December 1996     

Determination of nanoparticle sizes by X-ray diffraction

Different procedures for analysis of particle sizes by the X-ray diffraction method are compared by the example of nanoparticles of nickel and iron(3+) oxide (Fe₂O₃). A modified Warren-Averbach method is proposed for the analysis of the X-ray diffraction line profile based on the approximation by the Voigt function, which yields stable solutions, and the efficiency of the method is shown. The analysis within the frame-work of the Warren-Averbach method makes it possible to restore the distribution function of nanoparticles (crystallites) over true diameters, which satisfactorily correlates with electron microscopy data. The applicability of the Warren-Averbach method to the estimation of crystallite sizes by the analysis of a single diffraction line is substantiated. The range of the applicability of the Scherrer, Williamson-Hall, Warren-Averbach, and modified Warren-Averbach methods to the substructure analysis by the X-ray diffraction is determined as depending on the method of nanostructure formation.     

Atomic scattering factors for heavy atoms as investigated by small-angle gas electron diffraction

The experimental examination of the elastic and inelastic scattering factors for tin, iodine and mercury has been performed through the total-intensity     

Three-dimensional molecular packing of thin organic films of PTCDI-C8 determined by surface X-ray diffraction

We have determined the full molecular 3D packing of thin organic films of the archetypical organic n-type semiconductor N, N'-dioctyl-3,4:9,10-perylene tetracarboxylic diimide (PTCDI-C 8) by surface X-ray crystallography. We show that PTCDI-C 8 forms smooth layered films on Al 2O 3 (11-20) with an outstanding degree of molecular order. The thin-film structure is found to consist of a triclinic unit cell with the plane of the aromatic core tilted by 67 +/- 2 degrees with respect to the surface plane, which differs significantly from the bulk structure. The 3D crystallites extend with vertical coherent order across the entire film thickness.     

An investigation of the adiabatic potential energy surface of a Pseudo-Jahn-Teller complex using X-ray diffraction

X-ray diffraction combined with theoretical results obtained for isolated molecules can reveal many topologic features of the adiabatic potential energy surface (APS) of pseudo-Jahn-Teller Cu(II) complexes. Single-crystal x-ray results of acetatobis (1,10-phenanthroline)copper(II) perchlorate from 10 to 351 K are presented. The observed Cu-O bond length changes of 0.26 and 0.38 Å are rationalized in terms of a one-dimensional APS with two nonequivalent minima. The Silver and Getz model of vibronic coupling applied to the temperature variation of the Cu-O bond lengths is not obeyed. The actual structures of the conformers associated with the energy minima were determined from the x-ray data. A means of estimating the pseudo-Jahn-Teller radius using mean-square vibrational amplitudes along the Cu-O bonds is also discussed.     

X-ray crystal structure of a thiabenzene derivative

The first success of an X-ray analysis of a thiabenzene derivative, 1-benzoyl-2-methyl-2-thianaphthalene is described.     

X-ray diffraction and scanning electron microscopy studies of calcium carbonate electrodeposited on a steel surface

Calcium carbonate was deposited on a stainless steel surface with the use of an electrical potential of 10 V. The crystals formed on the surface were examined with X-ray diffraction and with scanning electron microscopy, which revealed that calcite, vaterite and amorphous calcium carbonate was formed. Two different surface active polymers were added to the solution and their effect on the crystal structure was investigated. It was found that the more hydrophilic of the two polymers promoted calcite growth and suppressed vaterite growth. The more hydrophobic polymer completely inhibited vaterite growth. Both polymers decreased the amount of crystals formed on the steel surface, the more hydrophobic polymer being the most effective. The crystal inhibition efficiency was enhanced close to the cloud point of the polymers. The results were compared with the effect of poly(acrylic acid), a commonly used antiscalant. It was found that poly(acrylic acid) was about as efficient as the more hydrophobic polymer in decreasing the amount of calcium carbonate. At higher concentrations of poly(acrylic acid), almost all of the calcium carbonate precipitated in the amorphous form.     

Pt oxide and oxygen reduction at Pt(111) studied by surface X-ray diffraction

The influence of the oxygen reduction reaction on the oxidation of Pt(111) is studied by surface X-ray diffraction. The oxygen reduction reaction does not significantly influence the place-exchange process during the initial stages of oxidation and there is no change in the onset potential and kinetics.     

Molecular gelation mechanism of maltodextrins investigated by wide-angle X-ray scattering

Thermally reversible maltodextrin gels are two-phase systems, composed of disc-like crystalline domains with a diameter of about 300 nm and regions containing amorphous polymer chains and water. The structure of the polysaccharide chains within the lamellae is that of the crystalline B-form of amylose, the polymer chains are arranged in double-stranded helices, which are packed in a hexagonal unit cell (a=b=1.85 nm, c (fiber repeat)=1.04 nm,=120). As revealed by measurements of the excess wide-angle X-ray scattering of the polysaccharide, gelation of the solutions is due to a partial crystallization of the polymer. In non-gelling maltodextrin solutions a crystallinity cannot be detected.     

Vapor phase inclusion of ferrocene and its derivative in a microporous metal-organic porous material and its structural characterization by single crystal X-ray diffraction

The inclusion of ferrocene and its derivative in metal-organic porous material MOF-5 is achieved by vapor diffusion; single-crystal X-ray diffraction studies using synchrotron radiation of ferrocene-loaded MOF-5 reveal well-ordered guest molecules packed into the pores.