The field of X-ray imaging and X-ray diffraction have been combined in a new technique called Tomographic Energy Dispersive Diffraction Imaging (TEDDI). This diffraction imaging technique allows 3D sample images to be obtained, non-destructively, where each imaged point contains the atomic structural information associated with its diffraction pattern. The main drawback of the TEDDI technique is the long collection times needed to produce the images. In order to overcome this obstacle the rapid TEDDI (rTEDDI) system has been developed at the University of Manchester's Material Science Centre. The research and development of rTEDDI has been the focus of this PhD thesis. A proof of concept for the rTEDDI imaging technique was obtained using thin samples on station 7.6 SRS Daresbury. In this case a first generation array collimator was used in conjunction with an energy resolving Si pixelated detector. Structural information such as lattice parameters, crystal system and phase identiffcation were obtained for metal, polymer and deer antler bone samples. The use of high Z semiconductor detector material was investigated in order to increase the potential of TEDDI for larger and more dense samples. To enable penetration of larger samples high energy X-rays needed to be utilized. In order to detect these higher energies with a good efficiency the detector media was changed from Si to CdZnTe (CZT).The second generation rTEDDI, using CZT as the detection media, was intended to be used under high flux/high energy synchrotron radiation conditions. Testing of the system under these conditions on station 16.3 SRS Daresbury showed an inability to produce diffraction imaging. An in depth investigation into detector and collimator array performance showed a two fold cause. The ERD2004 detector was unable to handle the high countrates experienced during high flux/high energy synchrotron radiation conditions. The MK1.2 collimator array was found to become partially transparent to X-ray energies around the absorption edge of W resulting in the swamping of the diffraction signal under high flux/high energy synchrotron radiation conditions. A new detector Application Specific Integrated Circuit (ASIC) design, developed by the detector division and the Rutherford Appleton Laboratory, and Data Aquisition (DAQ) system, developed by Aspect Systems, as well as a number of new collimator array designs were developed and tested. Testing of the new collimator array structures have shown positive results and the new HEXITECdetector which was designed to be able to handle high countrates, have shown an unprecedented inter pixel uniformity and energy resolution which have been attributed to the ASIC performance and the use of better quality CZT material.

Orientadores: Angelo Malachias de Souza, Eduardo Granado Monteiro da Silva / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Física Gleb Wataghin / Made available in DSpace on 2018-08-19T18:22:37Z (GMT). No. of bitstreams: 1 Pauli_Murielde_M.pdf: 18020420 bytes, checksum: ea0b8509035e788d8af363ac04130ca2 (MD5) Previous issue date: 2012 / Resumo: Esta dissertação trata do estudo estrutural e termodinâmico de sistemas orgânicos auto-organizados utilizando diferentes técnicas de espalhamento de raios-x. Multicamadas autoorganizadas de dois tipos de moléculas de ácidos fosfônicos foram analisadas: para o OPA [Ácido octadecilfosfônico - CH2(CH3)17PO(OH)2] e para o OcPA [Ácido octilfosfônico - CH2(CH3)7PO(OH)2]. Utilizando a fonte do Laboratório Nacional de Luz Síncrotron (LNLS) realizamos um conjunto de experimentos para investigar a organização lamelar e planar destas moléculas em função da temperatura. Medidas de difração convencional permitiram introduzir modelos de empilhamento capazes de identificar a coexistência de diferentes configurações de ordenamento e modificações nas mesmas em função da temperatura. Uma vez estabelecidos estes modelos fizemos uso da técnica de difração de raios-x dispersiva em energia, ainda pouco utilizada no Brasil, para obter informações detalhadas sobre o volume relativo de material ordenado com cada uma das configurações encontradas, identificando aquelas que são termicamente mais estáveis. O padrão de organização das moléculas no plano foi também investigado realizando-se medidas em geometria de transmissão de raios-x. Reunindo as informações descritas acima construímos um diagrama de fase ilustrando o ordenamento lamelar e planar das moléculas em função da temperatura. Além disso, fizemos um estudo do comportamento crítico das configurações de ordenamento nas vizinhanças da transição ordemdesordem para cada tipo de molécula e acerca da organização de curto e longo alcance das moléculas nas multicamadas. Os resultados preliminares são apresentados no fim deste trabalho / Abstract: This thesis comprises structural and thermodynamic studies on self-assembled organic systems using synchrotron x-ray scattering techniques. Multilayers obtained from selforganization of phosphonic acid molecules were analyzed for two different compounds: the octadecylphosphonic acid [OPA ¿ CH2(CH3)17PO(OH)2] and the octylphosphonic acid [OcPA ¿ CH2(CH3)7PO(OH)2]. Using the source of the Brazilian Synchrotron Light Laboratory (LNLS) we have performed an ensemble of experiments to investigate their lamellar and in-plane order of these molecules and their behavior. Conventional angle-resolved X-ray diffraction measurements were analyzed using kinematical models and allowed to verify the coexistence of distinct lamellar configurations as well as to track changes as the temperature rises. Once structural parameters were determined from the established models, detailed information about the relative volume of each lamellar configuration was retrieved using energy-dispersive X-ray diffraction, a technique still poorly explored in Brazil. This allowed identifying the most stable configurations at high temperatures. The in-plane order of molecules was also studied using x-ray transmission geometry via a wide-angle x-ray scattering setup. Gathering the above mentioned information we have built phase diagrams depicting the lamellar and planar packing of OPA and OcPA molecules as a function of temperature. Finally, we have performed a study of the critical behavior of the ordered configurations in the vicinity of order-disorder transition temperatures for each molecule. The preliminary results explained in the final chapter of this work shed light into the short- and long-range order behavior of the two systems / Mestrado / Física / Mestre em Física