Une nouvelle méthodologie d'analyse monocristalline par diffraction des rayons X (DRX) a été développée pour combler une lacune de l'analyse des contraintes d'ordre II (à l'échelle du grain) dans un matériau cristallin à structure non cubique. Cette méthode est basée sur la méthode d'Ortner I en introduisant le tenseur métrique qui lie le tenseur des déformations et les distances inter réticulaires mesurées par DRX. Avec cette nouvelle méthodologie, lorsque le repère cristallin direct n'est ni nécessairement orthogonal ni nécessairement normé, un repère orthonormé associé au repère cristallin direct est défini, où la majorité des calculs sont exécutés avec les règles de calcul usuelles. La méthode des moindres carrés nous permit de prise en compte de plus de 6 mesures minimum pour obtenir une meilleure estimation de G et déterminer les incertitudes statistiques. L'application expérimentale dans un bi cristaux cuivre nous a permit d'avoir validé cette nouvelle méthode. Par cette méthode, des contraintes résiduelles d'ordre II dans une couche galvanisé à gros grains sur l'acier sont déterminées après un traitement thermique de recuit. Les 4 grains orientés différemment sont été aussi quantitativement caractérisés in situ sous une sollicitation extérieure. Les résultats ont bien démontré le mécanisme de déformation élastique et plastique à l'échelle des grains et entre les grains. Par conséquent, cette méthode développée est donc adaptable et significative pour détermination des déformations et des contraintes à l'échelle des grains dans un monocristaux ou multicristaux à cristalline structure quelconque.

Nous avons étudié par des calculs de structure électronique ab initio la structure, la stabilité et la mobilité des lacunes, bilacunes et auto-interstitiels dans le zirconium hexagonal compact. La migration des mono-lacunes est légèrement plus rapide dans les plans de base et celle des bilacunes est isotrope et beaucoup plus rapide. Pour les auto-interstitiels, il existe une compétition entre sept configurations très proches en énergies, dont trois qui n'avaient pas été identifiées auparavant. Nos calculs suggèrent que la configuration basale octaédrique est la plus stable et que la migration est isotrope. Ce nouveau paysage énergétique, conforté par des simulations de dynamique moléculaire ab initio, permet de réconcilier calculs et expériences. Les autres métaux du groupe IVb, Ti et Hf, ont un comportement très semblable.

Mesoporous silica materials containing microporous cavities provided by covalently bound ¦Â-cyclodextrin (CD ICS) were synthesized by co-condensation of a ¦Â-CD functionalized triethoxy silane (CD ICL) with tetraethyl orthosilicate (TEOS) by using neutral amine surfactants as structure directing agents (SDA). CD ICL was prepared by reacting ¦Â-CD with 3-isocyanatopropyltriethoxysilane. IR spectroscopy of CD ICL showed complete disappearance of isocyanato group at 2270 cm-1. 1H NMR results indicate an average of four isocyanate linkers covalently attached to random hydroxyl substituents of each molecule of ¦Â-CD. <p> Nine different CD ICS materials were synthesized using dodecylamine, tetradecylamine or hexadecylamine with ¦Â-CD (2, 4, and 6 mol %) with respect to TEOS. The incorporation of ¦Â-CD within the mesoporous framework was supported by IR, Raman, MALDI TOF MS, solid state 13C NMR CP-MAS and TGA results. Small angle X-ray diffraction results showed a peak at 2¦È ¡Ö 2.20, supporting the presence of an ordered silica mesostructure framework. For materials with same CD loading, the surface area and pore volume doubled as the surfactant from dodecylamine to hexadecylamine. However, as the CD loading increased from 2% to 6%, the surface area decreases by a factor of ~ 1.5. <p>MALDI TOF mass spectrometry showed two peaks at m/z 1157 a.m.u. and 1173 a.m.u. for [¦Â-CD + Na]+ and [¦Â-CD + K]+ respectively due to desorption of ¦Â-CD from the walls of the silica matrix. The 13C NMR CP MAS results showed 13C signals in the region ¦Ä=60-110 ppm due to the nuclei of ¦Â-CD. CD ICS materials were found to be effective as a sorbent in both gas and aqueous phases, respectively. The sorption capacity (mmol/g) of p-nitrophenol increased from 61% to 84% with an increase of CD loading from 2% to 6% and as the alkyl chain length of the SDA increases from dodecylamine to hexadecylamine. The adsorption isotherm of CH3Cl in the gas phase and that of p-nitrophenol in the aqueous phase at ambient temperature adopts a multilayer model of adsorption.

Mesoporous silica materials containing microporous cavities provided by covalently bound ¦Â-cyclodextrin (CD ICS) were synthesized by co-condensation of a ¦Â-CD functionalized triethoxy silane (CD ICL) with tetraethyl orthosilicate (TEOS) by using neutral amine surfactants as structure directing agents (SDA). CD ICL was prepared by reacting ¦Â-CD with 3-isocyanatopropyltriethoxysilane. IR spectroscopy of CD ICL showed complete disappearance of isocyanato group at 2270 cm-1. 1H NMR results indicate an average of four isocyanate linkers covalently attached to random hydroxyl substituents of each molecule of ¦Â-CD. <p> Nine different CD ICS materials were synthesized using dodecylamine, tetradecylamine or hexadecylamine with ¦Â-CD (2, 4, and 6 mol %) with respect to TEOS. The incorporation of ¦Â-CD within the mesoporous framework was supported by IR, Raman, MALDI TOF MS, solid state 13C NMR CP-MAS and TGA results. Small angle X-ray diffraction results showed a peak at 2¦È ¡Ö 2.20, supporting the presence of an ordered silica mesostructure framework. For materials with same CD loading, the surface area and pore volume doubled as the surfactant from dodecylamine to hexadecylamine. However, as the CD loading increased from 2% to 6%, the surface area decreases by a factor of ~ 1.5. <p>MALDI TOF mass spectrometry showed two peaks at m/z 1157 a.m.u. and 1173 a.m.u. for [¦Â-CD + Na]+ and [¦Â-CD + K]+ respectively due to desorption of ¦Â-CD from the walls of the silica matrix. The 13C NMR CP MAS results showed 13C signals in the region ¦Ä=60-110 ppm due to the nuclei of ¦Â-CD. CD ICS materials were found to be effective as a sorbent in both gas and aqueous phases, respectively. The sorption capacity (mmol/g) of p-nitrophenol increased from 61% to 84% with an increase of CD loading from 2% to 6% and as the alkyl chain length of the SDA increases from dodecylamine to hexadecylamine. The adsorption isotherm of CH3Cl in the gas phase and that of p-nitrophenol in the aqueous phase at ambient temperature adopts a multilayer model of adsorption.

In this study, we investigate and fabricate two-dimensional ordered lattice structure by breath figures method. The breath figures pattern was prepared with the solution of carbon disulfide (CS2) doped with 1% weight concentration of polystyrene. The temperature and the humidity were controlled at ~23¢J and ~60 %, respectively. The breath figures pattern began to expand while CS2 is under evaporation. We explored the relationship between self-assemble of the water droplet and ordered structure via the solution height, the temperature evolution, and the dynamical optical images in the formation process of breath figures pattern. It was found that the radius of the water droplets varying with time follows the power law, £l ~ t £go; £g0=0.76. The fast Fourier transformation and Voronoi Diagram were used to conform that the formation of the breath figures pattern varied form a disordered state to an ordered state with the evaporation of CS2. The understanding of the breath figures pattern provides us to fabricate the photonics with size from nano- to micro-scale and to improve the application of nano device.

This study focuses on hexagonally sampled images and grayscale morphology. We combine hexagonal image processing and grayscale morphology to develop hexagonal grayscale morphology, and propose an algorithm to detect and enhance edges. Hexagonal image processing consists of three important steps: conversion of hexagonally sampled images, processing, and display of processed images on simulated hexagonal grid. We construct four different sizes of hexagonal structuring elements to apply morphological operations on hexagonal images. In this study, we applied morphological gradient for edge detection and proposed algorithm for edge enhancement. Moreover, we developed six different shapes of structuring elements to find an optimum one. Finally, we assessed two methods to compare our results, and identified the best result and optimum structuring element. We expect that proposed algorithm will offer a useful tool of image processing on hexagonally sampled images.

Hexagonal boron nitride (h-BN) formation by carbothermic reduction of B2O3 under nitrogen atmosphere at 1500&deg / C and effect of CaO addition into the initial B2O3 &amp / #8211 / active C mixture were investigated during this study. Reaction products were characterized by powder X-ray diffraction, scanning electron microscopy (SEM) and quantitative chemical analysis. Main aim of this study was to investigate the presence of a second reaction mechanism that catalytically affects h-BN formation during CaO or CaCO3 addition into the initial mixture. It was found that similar to CaCO3 addition, CaO addition has a catalytic effect on carbothermic formation h-BN. In order to investigate the reaction mechanism experiments with B2O3 &amp / #8211 / CaO mixtures without active carbon addition into the mixture were conducted. Furthermore nucleation of h-BN from calcium borate melts had been investigated and experiments were conducted with h-BN addition into CaO &amp / #8211 / B2O3 mixtures. It was concluded that nucleation of h-BN in calcium borate slags under experimental conditions is not possible. Hexagonal BN should be present in the system in order to activate the second nitrogen dissolution followed by h-BN precipitation mechanism. Highest efficiency was achieved in the experiment conducted with CaCO3 addition and largest particle size was observed during the experiment conducted to investigate the effect of nucleation.

Effect of Na2CO3 on formation of hexagonal boron nitride (h-BN) by carbothermic method has been studied by subjecting B2O3-C and Na2CO3-added B2O3-C mixtures to N2 (g) atmosphere. Na2CO3 amount in the mixtures was changed in the range of 0-40 wt. %. Time and temperature were used as experimental variables. Reaction products were analyzed by XRD and scanning electron microscope. Na2CO3 was found to increase both the amount and the particle size of h-BN similar to CaCO3 [1]. Na2CO3 was found to be less effective than CaCO3 in increasing the amount while it was more effective than CaCO3 in increasing the particle size of h-BN forming.

Carbothermic production of hexagonal BN by using boric acid and ground colemanite mined from Bigadi&ccedil / Region in Turkey was investigated by subjecting pellets prepared from B2O3, activated carbon and colemanite mixtures to nitrogen gas at 1500&deg / C. Similar to CaCO3 addition, colemanite addition to the B2O3-C mixtures resulted in higher amounts of h-BN in the final products. As a result of the experiments conducted with colemanite and CaCO3 additions providing the same quantity of CaO to the initial mixtures, similar amounts of hexagonal BN in the reaction products were observed. As a result of the experiments conducted with different compositions of colemanite- B2O3- C mixtures, 5 wt % colemanite addition was determined to be the optimum composition giving the highest amount of hexagonal BN in the reaction products. Increasing duration of the experiments increased the amount and particle size of h-BN formed in the products. Optimum amount of colemanite addition resulted in higher amounts and coarser particles of h-BN in the products than the optimum amounts of CaCO3 addition.

Thermal behavior and molecular packing of a series of £\-helical poly(L-glutamates), with n-alkyl side chain of various lengths (m(number of carbons in the alkyl group) = 1, 2, 6, 12,18), were studied by means of differential scanning calorimetry, polarizing light microscopy and X-ray diffraction. For polymers of m = 1 and 2, There is a pseudohexagonal structure below ca. 130 oC and above this temperature the stable phase is the hexagonal columnar phase. There exists a layered structure in the polymer of m = 6, as well as a solvent induced hexagonal columnar structure which formed during solution casting process. In the polymer of m = 12, a layered structure was formed in the temperature range between 20 to 255 oC. However, for longer side chain, m = 18, tendency of crystallization of alkyl long side chain forced the backbone to pack into layer structure. There are two distinct melting temperature at ca. 60 oC, and the enthalpy are ca. 53 and 19 J/g, which corresponding to the melting of hexagonal and monoclinic side chain crystallines. The polymers with longer side chain (m = 6, 12 and 18) tend to be lyotropic liquid crystalline phase within lamellar inter-rod distance of 1.25 nm in solution state, and the structure will remain after drying. However, the inter-rod distance will collapse at the temperature above ca. 200 ¢J and will not recover after cooling.