Depuis l'arrêt définitif des essais nucléaires, la Direction des Applications Militaires (DAM) du CEA s'appuiesur le triptyque modélisation physique - validation expérimentale - simulation numérique pour comprendre,prévoir et garantir le fonctionnement des armes nucléaires. Parmi les grands équipements contribuant à lavalidation des modèles physiques implémentés dans les logiciels de calcul, le Laser MegaJoule permetd'étudier expérimentalement des phénomènes de même nature que ceux intervenant dans les armes. La familled'objets expérimentés sur cette installation est dénommée « microcibles laser». Les microballons intégrés dansces microcibles sont caractérisés par des techniques de radiographie X. Les brusques variations de niveau degris observées sur les clichés X de microballons témoignent de la 'présence d'un phénomène de contraste dephase, contraste s'ajoutant au contraste d'absorption. L'information contenue dans ce phénomène est utiliséepour une détection de contours du microballon radiographié. Les points trouvés lors de la détection de contourssont alors utilisés par un algorithme d'estimation des défauts de formes des surfaces des microballons. Uneétude paramétrique permet d'identifier le nombre de clichés nécessaire à l'estimation des défauts de forme enfonction du nombre de modes souhaités. L'incertitude de la méthode d'estimation est calculée permettant lacaractérisation complète du microballon. / Since 1996, the CEA's Military Applications Division (DAM) guaranties the reliability and safety of Frenchnuclear warheads without conducting any further nuclear test. It relies particularly on major facilities forvalidating the equations used to model the functioning of nuclear weapons. Among them, the Megajoule Laser(LMJ) allows studying experimentally, as "laboratory" measurements, representative phenomena gatheringtime·scale and space distribution of extreme temperature and pressure conditions. These experiments are ledwith millimetric objects named microshells. Before experimenting them, these microshells are characterizedusing X·rays technics. On the radiographies, one can observe straight gray level variations which are generatedby the phase contrast phenomenon added to x·rays absorption contrast. Information included in this formercontrast is used to sharply determine microshell's edges. The delimiting points of these edges are thenintegrated as input data to compute microshell's surface form defects. A study is also led to determine theoptimized number of radiographies needed for estimating the search defect modes. Measurement uncertainty isfinally evaluated, thus giving a complete microshell's characterization.

This thesis is an experimental investigation of phase behavior, crystallization, gelation and phase separation kinetics of polymer solutions in dense fluids at high pressures. The miscibility and dynamics of phase separation were investigated in solutions of atactic polystyrene with low polydispersity (Mw = 129,200; PDI = 1.02) in acetone. Controlled pressure quench experiments were conducted at different polymer concentrations to determine both the binodal and the spinodal envelops using time- and angle resolved light scattering techniques. At each concentration, a series of rapid pressure quenches with different penetration depths in a range from 0.1 MPa to 3 MPa were imposed and the time evolution of the angular distribution of the scattered light intensities was monitored. The solution with 11.4 wt % polymer concentration underwent phase separation by spinodal decomposition mechanism for both shallow and deep quenches. Below this critical polymer concentration, phase separation was found to proceed by nucleation and growth mechanism for shallow quenches, but by spinodal decomposition for deeper quenches. Gelation and crystallization processes and the influence of pressure and the fluid [Cho et al. 1993]composition were investigated in solutions of poly(4-methyl-1-pentene) [P4MP1] in n-pentane + CO₂ and in solutions of syndiotactic polystyrene [sPS] in toluene + CO₂, and also in acetophenone + CO₂ fluid mixtures over a pressure range up to 55 MPa and carbon dioxide levels up to 50 wt %. In pure pentane, P4MP1 undergoes crystallization and leads to Form III polymorph at low pressures, but to Form II at high pressures. In n-pentane + CO₂ mixture fluids, the polymorphic state changes from a mixture of Forms III and II to Form II and eventually to Form I with increasing CO₂ content. High level of carbon dioxide (≥40 wt %) in the solution was found to lead to gelation instead of crystallization. No liquid-liquid phase boundaries could be observed in any of the P4MP1 solutions. In contrast to P4MP1 in n-pentane, syndiotactic polystyrene was found to undergo gelation in toluene or acetophenone forming a polymer-solvent compound with the δ crystal form. Also in contrast to P4MP1 systems, addition of carbon dioxide to sPS solutions alters the process from that of gelation to crystallization leading to the β crystal form. In solutions with high CO₂ level, in addition to the gelation or crystallization boundaries, a liquid-liquid phase separation boundary was also observed. The phase separation path followed was found to influence the eventual morphology and the crystal state of the polymer. In sPS solutions in toluene + CO₂, if the sol-gel boundary were crossed first by cooling the solution at a fixed pressure, the resulting morphology was found to be fibrillar and the polymer displayed the δ crystal form. If instead, the liquid—liquid phase boundary were crossed first by reducing pressure at a fixed temperature, the polymer-rich phase leads to a stacked-lamellar morphology with the β crystal form while the polymer-lean phase leads to a mixed morphology with lamellar layers connected by fibrils with the polymer displaying δ + β crystal forms. In solutions in acetophenone + carbon dioxide, when the gelation boundary is crossed first, the resulting structure is the δ form as in the toluene + CO₂ case. At comparable CO₂ levels, when the L-L phase boundary is crossed first, in the acetophenone system, polymer-rich phase was found to generate a mixture of δ + β forms while only the δ form was found in the polymer-lean phase, in contrast to the observations in the toluene + CO₂ systems. Based on crystallographic, spectral and microscopic data, a thermodynamic framework was developed which provides a mechanistic account for the formation of the different polymorphs. / Ph. D.

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