The object of this thesis is to apply scanning probemicroscopy (SPM) to the field of advanced powder processing.Measurement of interparticle surface forces at conditionsrelevant to ceramic processing has been performed together withthorough studies of powder friction. Surface force measurements between silicon nitride andsilica surfaces in 1-bromonaphtalene and diiodomethane resultedin an attractive van der Waals force in both media for thesymmetric systems and a repulsive van der Waals force for theasymmetric systems. This agreed well with theoreticalpredictions from Lifshitz theory. Measurements in electrolytesolutions between silicon nitride surfaces with a varyingdegree of oxidation showed that silanol groups dominated theinteractions at a high degree of oxidation, whereas theinfluence of amine species became stronger after surfaceetching. Surface charge, surface potential and density ofsurface groups have been extracted from DLVO computer modellingof the experimental force curves. Surface force measurementshave been carried out using a nitrided silica sphere as acolloidal probe, representative for commercial silicon nitridepowders. Adsorption of poly(acrylic acid) above the isoelectricpoint generated a thin polymer layer of an essentially flatconformation. Friction force measurements were attainable via novelcalibration procedures of both the lateral photodetectorresponse and the cantilever torsional spring constant.Combining the method for detector calibration with evaluationof static friction slopes simplified the choice of appropriatecontact mechanics theory to evaluate the friction measurements.Applying the method on friction measurements between ironsurfaces coated with commercial lubricants showed a substantialsurface deformation not seen from the friction force alone. Thenanorheological properties of silica surfaces coated with twodifferent stearic acids have been evaluated from friction forcemeasurements. Steady sliding motion was replaced by highlyregular stick-slip motion at a critical load and velocity. Thestick-slip motion was successfully described and fitted to aphenomenological model. The contact area evaluated fromMaugis-Dugdale theory revealed the contact diameter to be veryclose to the stick-slip periodicity. Friction measurements were carried out between individualspray-dried ceramic granules as a function of binderconcentration and relative humidity. The hygroscopic nature ofthe binder resulted in a higher adhesion force but lowerfriction coefficient with increasing humidity. This effect wasascribed to softening of the binder and a lowering of the shearstrength of the binder rich surface layer on the granules.Comparison of the friction force between two granules and agranule and a hard metal surface confirmed that resistance toflow during the initial stages of powder pressing is dominatedby granule-wall friction and adhesion. Keywords: Atomic force microscope, AFM, SPM, van der Waalsinteraction, DLVO-theory, surface forces, colloidal probe,force curve, friction, adhesion, stick-slip, cantilever,calibration, spring constant, silicon nitride, iron,silica.

<p>The object of this thesis is to apply scanning probemicroscopy (SPM) to the field of advanced powder processing.Measurement of interparticle surface forces at conditionsrelevant to ceramic processing has been performed together withthorough studies of powder friction.</p><p>Surface force measurements between silicon nitride andsilica surfaces in 1-bromonaphtalene and diiodomethane resultedin an attractive van der Waals force in both media for thesymmetric systems and a repulsive van der Waals force for theasymmetric systems. This agreed well with theoreticalpredictions from Lifshitz theory. Measurements in electrolytesolutions between silicon nitride surfaces with a varyingdegree of oxidation showed that silanol groups dominated theinteractions at a high degree of oxidation, whereas theinfluence of amine species became stronger after surfaceetching. Surface charge, surface potential and density ofsurface groups have been extracted from DLVO computer modellingof the experimental force curves. Surface force measurementshave been carried out using a nitrided silica sphere as acolloidal probe, representative for commercial silicon nitridepowders. Adsorption of poly(acrylic acid) above the isoelectricpoint generated a thin polymer layer of an essentially flatconformation.</p><p>Friction force measurements were attainable via novelcalibration procedures of both the lateral photodetectorresponse and the cantilever torsional spring constant.Combining the method for detector calibration with evaluationof static friction slopes simplified the choice of appropriatecontact mechanics theory to evaluate the friction measurements.Applying the method on friction measurements between ironsurfaces coated with commercial lubricants showed a substantialsurface deformation not seen from the friction force alone. Thenanorheological properties of silica surfaces coated with twodifferent stearic acids have been evaluated from friction forcemeasurements. Steady sliding motion was replaced by highlyregular stick-slip motion at a critical load and velocity. Thestick-slip motion was successfully described and fitted to aphenomenological model. The contact area evaluated fromMaugis-Dugdale theory revealed the contact diameter to be veryclose to the stick-slip periodicity.</p><p>Friction measurements were carried out between individualspray-dried ceramic granules as a function of binderconcentration and relative humidity. The hygroscopic nature ofthe binder resulted in a higher adhesion force but lowerfriction coefficient with increasing humidity. This effect wasascribed to softening of the binder and a lowering of the shearstrength of the binder rich surface layer on the granules.Comparison of the friction force between two granules and agranule and a hard metal surface confirmed that resistance toflow during the initial stages of powder pressing is dominatedby granule-wall friction and adhesion.</p><p>Keywords: Atomic force microscope, AFM, SPM, van der Waalsinteraction, DLVO-theory, surface forces, colloidal probe,force curve, friction, adhesion, stick-slip, cantilever,calibration, spring constant, silicon nitride, iron,silica.</p>

Στόχος της παρούσας διδακτορικής διατριβής είναι η μελέτη χρονικά μεταβαλλόμενων και ασταθών υπό συνθήκες ροών ιξωδοπλαστικών και ιξωδο-ελαστικών ρευστών λόγω της σημασίας που παρουσιάζουν τα υλικά αυτά σε διάφορες βιομηχανικές διεργασίες. Στα πλαίσια της εργασίας αυτής μελετήθηκε αρχικά το πρόβλημα της συμπίεσης ιξωδοπλαστικού ρευστού μεταξύ δύο δίσκων το οποίο είναι ένα βασικό πείραμα ρεολογικού χαρακτηρισμού μη Νευτωνικών υλικών. Η χρονικά μεταβαλλόμενη προσομοίωση επέτρεψε τον προσδιορισμό των σημαντικών διαφορών μεταξύ των δύο εκδοχών του συγκεκριμένου ρεολογικού πειράματος (δίσκοι κινούμενοι υπό σταθερή ταχύτητα ή υπό σταθερή δύναμη) που ήταν αδύνατος με τα προηγούμενα μοντέλα, ενώ παρουσιάζεται και πλήρης παραμετρική μελέτη της διεργασίας αυτής. Το υπόλοιπο μέρος της παρούσας εργασίας αφιερώθηκε στη μελέτη της διεργασίας εκβολής ιξωδοελαστικών υλικών η οποία συναντάται ευρέως στη βιομηχανία μορφοποίησης πολυμερών. Παρουσιάζεται μια πλήρης παραμετρική ανάλυση για την εκβολή ενός ιξωδοελαστικού ρευστού Phan-Tien & Tanner (PTT) από ένα δακτυλιοειδή αγωγό προκειμένου να εξετάσουμε την επίδραση της γεωμετρίας του αγωγού, και των ρεολογικών ιδιοτήτων του ρευστού. Επιπλέον ένα σημαντικό πρόβλημα που εμφανίζεται κατά την εκβολή από ένα κυλινδρικό, επίπεδο ή δακτυλιοειδή αγωγό είναι η εμφάνιση ασταθειών οι οποίες επηρεάζουν σημαντικά την ποιότητα του τελικού προϊόντος. Προκειμένου να διερευνηθεί ο μηχανισμός που προκαλεί την εμφάνιση αυτών των ασταθειών πραγματοποιήθηκε γραμμική ανάλυση ευστάθειας για τη αξονοσυμμετρική και καρτεσιανή δισδιάστατη ροή επικόλλησης-ολίσθησης (stick-slip flow) ενός ρευστού PTT. Γύρω από τη λύση μόνιμης κατάστασης πραγματοποιείται γραμμική ανάλυση ευστάθειας, και υπολογίζονται οι ιδιοτιμές του γενικευμένου προβλήματος με τη βοήθεια της μεθόδου Arnoldi. Έτσι προσδιορίζεται η επίδραση των ιδιοτήτων του υλικού στην ευστάθεια ή μη της ροής. / The purpose of this dissertation is to perform a study on time-dependent and conditionally unstable flows of viscoplastic and viscoelastic fluids because of their importance in various industrial processes. A typical experiment which is used widely for the rheological characterization of non-Newtonian fluids is squeeze flow which is the subject of the first chapter of this dissertation. The time-dependent simulation permitted the determination of the distinct differences between the two versions of this rheological experiment (disks moving with constant velocity or under constant force) which was impossible with the models used up to now, while a complete parametric analysis of this process is presented. The rest of this work focuses in the important problem of the extrusion process of a viscoelastic fluid, which is frequently encountered in the polymer industry. A complete parametric analysis is presented for the extrusion of a Phan-Thien Tanner (PTT) fluid from an annular die in order to examine the effect of the die geometry and the rheological properties of the fluid on this process. Moreover, it is widely known that during the extrusion from a cylindrical, planar or an annular die various flow instabilities may arise affecting significantly the quality of the final product. In order to investigate the mechanism, which causes the appearance of these instabilities, a linear stability analysis is performed for the cylindrical or planar stick-slip flow of a PTT fluid. The stability analysis is performed around the steady state solution and the eigenvalues of the generalized problem are calculated using the Arnoldi algorithm. With this method the effect of the various rheological properties of the fluid on the stability of the flow is determined.

No description available.

An experimental evaluation of the mixed-mode fracture behavior of bonded composite joints is presented. Commonly used experimental techniques for characterizing the mode I, mixed-mode I/II, mode II, and mode III fracture behavior have been employed for the purpose of developing a fracture envelope to be utilized in the automotive design process. These techniques make use of such test geometries as the double cantilever beam (DCB), asymmetric double cantilever beam (ADCB), single-leg bend (SLB), end-loaded split (ELS), and split cantilever beam (SCB) specimens. Symmetric versions of the DCB, SLB, and ELS specimens produced mode mixities of 0°, 41°, and 90° respectively, while the testing of ADCB specimens allowed for mode mixities of 18°, 31°. Pronounced stick-slip behavior was observed for all specimen test geometries under both quasi-static and dynamic loading conditions. Due to the nature of the adhesive studied, a limited number of data points were obtained under mode I loading conditions. A significant increase in the number of measurable crack initiation events was observed for mixed-mode I/II loading conditions, where stick slip behavior was less pronounced. Additionally, a comparison of the measured fracture energies obtained under mixed-mode I/II loading conditions reveals that the addition of a small mode II component results in a decrease in the mode I fracture energy by roughly 50%, as the crack was driven to the interface between the adhesive layer and composite adherends. Furthermore, the propensity of debonds to propagate into the woven composite laminate adherends under mode II loading conditions limited the number of crack initiation points that could be obtained to one or two usable data points per specimen. A limited number of experimental tests using the SCB specimen for mode III fracture characterization, combined with a numerical analysis via finite element analysis, revealed a significant mode II contribution toward the specimen edges. Similarly, FE analyses on full bond width and half bond width SCB specimens was conducted, and results indicate that by inducing a bond width reduction of 50%, the mode II contribution is greatly decreased across the entire width of the specified crack front. To provide a means for comparison to results obtained using the standard DCB specimen, an alternative driven wedge test specimen geometry was analyzed, as this geometry provided a significant increase in the number of measurable data points under mode I loading conditions. A three-dimensional finite element analysis was conducted to establish ratios of simple beam theory results to those obtained via FEA, GSBT/GFEA, were of particular interest, as these ratios were used to establish correction factors corresponding to specific crack lengths to be used in correcting results obtained from an experimental study utilizing a driven wedge technique. Corrected results show good agreement with results obtained from traditional mode I double cantilever beam tests. Finally, bulk adhesive experiments were conducted on compact tension specimens to establish a correlation between adhesively bonded composite joint and bulk adhesive fracture behavior under mode I loading conditions. Measured fracture energy values were shown to gradually drop across a range of applied loading rates, similar to the rate-dependent behavior observed with both the DCB and driven wedge specimens. Application of the time-temperature superposition principle was explored to determine whether or not such techniques were suitable for predicting the fracture behavior of the adhesive studied herein. Good correlation was established between the fracture energy values measured and the value of tan d obtained from dynamic mechanical analysis tests conducted at corresponding reduced test rates. / Master of Science

La spectroscopie électronique basée sur l'effet tunnel donne accès à la densité d'états des électrons (DoS) dans les matériaux conducteurs, et renseigne ainsi en détail sur leurs propriétés électroniques. <br />Au cours de cette thèse, nous avons développé un microscope permettant d'effectuer la spectroscopie tunnel résolue spatialement (10 nm) de nanocircuits individuels, avec une résolution en énergie inégalée (10 µeV). Cet appareil combine les fonctions de Microscopie par Force Atomique (mode AFM) et de spectroscopie Tunnel locale (mode STM), et fonctionne à 30 mK. Dans le mode AFM, la topographie de l'échantillon est imagée grâce à un diapason en quartz piézoélectrique, ce qui permet de repérer les circuits. La spectroscopie tunnel peut ensuite être faite sur les zones conductrices. <br />Avec ce microscope, nous avons mesuré la DoS locale dans une structure hybride Supraconducteur-métal Normal-Supraconducteur (S-N-S). Dans un tel circuit, les propriétés électroniques de N et de S sont modifiées par l'effet de proximité supraconducteur. Notamment, pour des fils N courts, nous avons pu observer -comme prédit- la présence d'un gap dans sa DoS, indépendant de la position dans la structure : le “minigap”. De plus, en modulant la phase supraconductrice entre les deux S, nous avons mesuré la modification de ce gap, et sa disparition lorsque la différence de phase vaut π. <br />Nos résultats expérimentaux pour la DoS, ainsi que ses dépendances en phase, en position, et en longueur de N sont en accord quantitatif avec les prédictions de la théorie quasiclassique de la supraconductivité. Certaines de ces prédictions sont observées pour la première fois.

Cette étude a pour objectifs la caractérisation expérimentale des frottements saccadés dans les matériaux granulaires modèles constitués des billes de verre monodisperses en compression triaxiale drainée et l'identification des paramètres de contrôle. Cinq paramètres macroscopiques caractérisent ces frottements saccadés : la chute de déviateur et la contraction volumique, l'intermittence de déformation axiale, le module d'Young et le coefficient de Poisson. Les frottements saccadés affectent simultanément le déviateur et la déformation volumique. Le comportement macroscopique est globalement contractant tandis que le matériau tend vers un état limite critique en grandes déformations, à la manière des sables lâches. Cependant il présente localement, dans les phases de blocage qui suivent immédiatement les ruptures temporaires, le comportement dilatant des sables denses, qui obéit à une relation contrainte-dilatance linéaire et unique. Les frottements saccadés disparaissent au-delà d'une vitesse critique d'écrasement axial, qui dépend de la contrainte de confinement et de la taille des grains. Le module d'Young dynamique par propagation d'ondes varie avec la contrainte de confinement selon une loi de puissance. Le module d'Young quasi-élastique au départ des phases de blocage est constant à l'intérieur du domaine élastique, de même que le coefficient de Poisson. Le suivi par granulométrie laser et par analyse d'images des matériaux après un ou plusieurs essais triaxiaux permet de suivre l'évolution de la taille moyenne et de la forme des grains. Tandis que les instabilités par saccade disparaissent suite à un certain nombre d'essais, on observe, simultanément à une légère diminution du volume moyen, l'apparition progressive de populations d'objets non sphériques par une fusion des grains analogue au frittage. / The objectives of this study are the experimental characterisatino of the stick-slip instabilities in a model granular material and the identification of relevant control parameters. As monodisperse glass beads are subjected to drained triaxial compression tests, five macroscopic parameters characterize the stick-slip phenomenon: the deviator drop, the jump in volumetric contraction, the intermittence of the axial strain, Young’s modulus and Poisson’s ratio. The stick-slip events simultaneously affect the deviator stress and the volumetric strain. While the global material behavior is that of a loose sand, gradually contracting and hardening as it approaches its large strain critical state, its response in the “stick” phases immediately following the “slip” instabilities is similar to that of dense, dilatant sands, with a unique, linear stress-dilatancy relationship. Stick-slip events disappear beyond a critical axial strain rate, depending on the confining stress and on the grain diameter. The Young modulus associated to wave propagation varies with the confining stress according to a power law. The quasi-elastic modulus measured at the beginning of the stick phase is constant inside the elastic domain, as well as the Poisson ratio. The evolution of grain size and shape after one or several triaxial tests is monitored by laser granulometry and image analysis. The gradual vanishing of stick-slip events, on repeating the tests, is likely related to the global decreasing trend of average particle volume and to the formation of non-spherical objects, apparently by some phenomenon analogous to sintering.

近年，IoTに基づく「つながる工場」に関する技術開発が着目され，日本の次世代の製造業を支えるために，新しい研究開発が求められている．特に機械加工の現場では，異常検知や適応制御のために加工現象を精確かつリアルタイムにモニタできる技術が必要とされている．そこで，マシニングセンタなどの工作機械において，回転工具の加工中に多チャンネルで各種の物理量を切削点近傍にてモニタ可能な無線多機能ホルダを開発し，様々な工具，加工方法を対象にその有効性を示した． / Currently, a smart monitoring technology has been attracting particular attention in the factory automation fields regarding the Internet of things (IoT). Particularly in the machining site, the technology of monitoring the processing phenomenon in precision and real-time is required for abnormality detection or adaptive control. Then, we developed a novel tool holder equipped with a wireless communication function to monitor the tool temperature and vibrating accelerations near the cutting point during a tool rotating operation, and we showed effectiveness for various tools and processing method. / 博士(工学) / Doctor of Philosophy in Engineering / 同志社大学 / Doshisha University