Abstract: This work presents a new carbonsilica hybrid material, denoted as CSM, with remarkable sorption properties. It consists of intraporous graphitic nanocrystals grown in the pores of mesoporous silica. CSM is obtained by a subtle incipient wetness impregnation of Al-containing mesoporous silica with furfuryl alcohol (FA)/hemelitol solutions. Both the volume match of the impregnation solution with that of the silica template pore volume, and the presence of Al3+ in the silica, are crucial to polymerize FA selectively inside the mesopores. Carbonization of the intraporous polymer was then performed by pyrolysis under He up to 1273 K. The resulting CSMs were examined by SEM, HRTEM, 27Al MAS NMR, N2 adsorption, XRD, TGA, TPD, XPS, pycnometry and Raman spectroscopy. Mildly oxidized graphitic-like carbon nanoblocks, consisting of a few graphene-like sheets, were thus identified inside the template mesopores. Random stacking of these carbon crystallites generates microporosity resulting in biporous materials at low carbon content and microporous materials at high carbon loadings. Very narrow pore distributions were obtained when pyrolysis was carried out under slow heating rate, viz. 1 K min−1. Adsorption and shape selective properties of the carbon filled mesoporous silica were studied by performing pulse chromatography and breakthrough experiments, and by measuring adsorption isotherms of linear and branched alkanes. Whereas the parent mesoporous silica shows unselective adsorption, their CSM analogues preferentially adsorb linear alkanes. The sorption capacity and selectivity can be adjusted by changing the pore size of the template or by varying the synthesis conditions. A relation between the carbon crystallites size and the shape selective behaviour of the corresponding CSM for instance is demonstrated. Most interestingly, CSM shows separation factors for linear and branched alkanes up to values comparable to those of zeolitic molecular sieves.

Abstract: High-quality single crystals of Rb2ZnCl4 and K2ZnCl4, pure or doped with Cu, Mn, Cd, Tl, Sn, Pb and In cations, were grown by Czochralski technique in argon atmosphere, using an experimental setup that allows direct visual access to the whole growth zone. Slowly cooled crystals exhibit excellent cleavage properties. Fastly cooled crystals do cleave poorly. As shown by X-ray diffraction studies, such K2ZnCl4 samples exhibit inclusions of the high-temperature Pmcn phase with lattice parameters a = 7.263(2) Angstrom, b = 12.562(2) Angstrom and c = 8.960(4) Angstrom in the P2(1) cn room temperature stable phase. ESR and optical spectroscopy studies revealed the localization and valence state of the cation dopants. (C) 1999 Elsevier Science B.V. All rights reserved.

Abstract: This HREM investigation focuses on the influence of point defects on the final epitaxial relation and atomic interface configuration in a CoSi2/Si(1 0 0) heterostructure. A two-step SPE-MBE grown CoSi2/Si(1 0 0) system is used and, by altering the number of deposited Co monolayers in the template layer, the point defect behavior is studied. We propose a film growth model in which the knowledge about the reconstructed (2 x 1) : Si(1 0 0) surface, the point defect behavior in the presence of an interface, especially a silicide interface, the migration of point defects through a lattice by formation of [1 0 0]-split interstitial (dumbbell) atomic configurations, and a new type of extended defect configurations in diamond type materials will all amalgamate. (C) 1998 Published by Elsevier Science B.V. All rights reserved.

Abstract: In this paper, it has been investigated how to measure atom column positions as accurately and precisely as possible using a focal series of images. In theory, it is expected that the precision would considerably improve using a maximum likelihood estimator based on the full series of focal images. As such, the theoretical lower bound on the variances of the unknown atom column positions can be attained. However, this approach is numerically demanding. Therefore, maximum likelihood estimation has been compared with the results obtained by fitting a model to a reconstructed exit wave rather than to the full series of focal images. Hence, a real space model-based exit wave reconstruction technique based on the channelling theory is introduced. Simulations show that the reconstructed complex exit wave contains the same amount of information concerning the atom column positions as the full series of focal images. Only for thin samples, which act as weak phase objects, this information can be retrieved from the phase of the reconstructed complex exit wave.

Abstract: It has often been stated that a holographic biprism represents a near perfect energy filter and only elastically scattered electrons can participate in the interference fringes. This is based on the assumption that the reference wave does not contain inelastically scattered electrons. In this letter we show that this is not exactly true because of the delocalised inelastic interaction of the reference wave with the sample. We experimentally and theoretically show that inelastic scattering plays a role in the fringe formation, but it is shown that this contribution is small and can usually be neglected in practice. (C) 2011 Elsevier B.V. All rights reserved.

Abstract: The electronic properties of quaternary AlInGaN devices significantly depend on the homogeneity of the alloy. The identification of compositional fluctuations or verification of random-alloy distribution is hence of grave importance. Here, a comprehensive multiprobe study of composition and compositional homogeneity is presented, investigating AlInGaN layers with indium concentrations ranging from 0 to 17 at% and aluminium concentrations between 0 and 39 at% employing high-angle annular dark field scanning electron microscopy (HAADF STEM), energy dispersive X-ray spectroscopy (EDX) and atom probe tomography (APT). EDX mappings reveal distributions of local concentrations which are in good agreement with random alloy atomic distributions. This was hence investigated with HAADF STEM by comparison with theoretical random alloy expectations using statistical tests. To validate the performance of these tests, HAADF STEM image simulations were carried out for the case of a random-alloy distribution of atoms and for the case of In-rich clusters with nanometer dimensions. The investigated samples, which were grown by metal-organic vapor phase epitaxy (MOVPE), were thereby found to be homogeneous on this nanometer scale. Analysis of reconstructions obtained from APT measurements yielded matching results. Though HAADF STEM only allows for the reduction of possible combinations of indium and aluminium concentrations to the proximity of isolines in the two-dimensional composition space. The observed ranges of composition are in good agreement with the EDX and APT results within the respective precisions.

Abstract: Inelastic image simulation software is presented, implementing the double channeling approximation which takes into account the combination of multiple elastic and single inelastic scattering in a crystal. The approach is described with a density matrix formalism. Two applications in high resolution energy filtered (EFTEM) transmission electron microscopy (TEM) images are presented: thickness-defocus maps for SrTiO3 and exit plane intensities for an (LaAlO3)3(SrTiO3)3 multilayer system. Both systems show a severe breakdown in direct interpretability which becomes worse for higher acceleration voltages, thicker samples and lower excitation edge energies. Since this effect already occurs in the exit plane intensity, it is a fundamental limit and image simulations in EFTEM are indispensable just as they are indispensable for elastic high resolution TEM images.

Abstract: A new method for including higher-order Laue zones (HOLZs) effects in an efficient way in electron scattering simulations has been developed and tested by detail calculations. The calculated results by the conventional multislice (CMS) method and the improved conventional multislice (ICMS) method using a large dynamical aperture to avoid numerical errors are compared with accurate results. We have found that the zero-order Laue zones (ZOLZs) reflection cannot be properly described only using the projected potential in the whole unit cell; in general, we need to subslice the electrostatic potential inside the unit cell. It is shown that the ICMS method has higher accuracy than the CMS method for the calculation of the ZOLZ, HOLZ and Pseudo-HOLZ reflections. Hence, ICMS method allows to use a larger slice thickness than the CMS method and reduces the calculation time. (C) 2012 Elsevier B.V. All rights reserved.

Abstract: Homogenised and quenched Ni65Al35 samples were heated and studied in situ in a CM20 electron microscope up to 900 degrees C. The Ni5Al3 phase first forming around 550 degrees C in the quenched L1(0) microtwinned martensite starts to decompose around 800 degrees C yielding B2 precipitates in a twinned L1(2) matrix. The latter twinning is a remainder of the microtwinning in the original room temperature martensite. Also the crystallographic relations between precipitates and matrix can be traced back to the original formation of twinned martensite plates within the austenite. Some aspects of the dynamics of the process are discussed on the basis of snap shots and video recordings.

Abstract: Using a combination of electron holography and energy filtering, interference fringes produced after inelastic interaction of electrons with hydrogen molecules are examined. Surprisingly, the coherence of inelastic scattering increases when moving from the surface of a hydrogen-containing bubble to the vacuum. This phenomenon can be understood in terms of the Feynman two-slit thought experiment with a variable ambiguity of the which-way registration. (C) 2006 Elsevier B.V. All rights reserved.