In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.
The production of II -VI semiconductor compound -polymer matrix nanocomposites by a direct in-situ thermolysis process is described. Metal-thiolate precursor molecules embedded in a polymer matrix decompose by a thermal annealing and the nucleation of semiconductor nanocrystals occurs. It is shown that the nucleation of nanoparticles and the formation of the nanocomposite can be also achieved by laser beam irradiation; this opens the way towards a "lithographic" in-situ nanocomposite production process. A possible growth and nanocomposite formation mechanism, describing the structural and chemical transformation of the precursor molecules, their decomposition and the formation of the nanoparticles, is presented.
Coronary Heart Disease (CHD) is one of the leading causes of death worldwide, claiming over seven million lives each year. Permanent metal stents, the current standard of care for CHD, inhibit arterial vasomotion and induce serious complications such as late stent thrombosis. Bioresorbable vascular scaffolds (BVSs) made from poly L-lactide (PLLA) overcome these complications by supporting the occluded artery for 3-6 months and then being completely resorbed in 2-3 years, leaving behind a healthy artery. The BVS that recently received clinical approval is, however, relatively thick (~150 µm, approximately twice as thick as metal stents~80 µm). Thinner scaffolds would facilitate implantation and enable treatment of smaller arteries. The key to a thinner scaffold is careful control of the PLLA microstructure during processing to confer greater strength in a thinner profile. However, the rapid time scales of processing (~1 s) defy prediction due to a lack of structural information. Here, we present a custom-designed instrument that connects the strain-field imposed on PLLA during processing to in situ development of microstructure observed using synchrotron X-ray scattering. The connection between deformation, structure and strength enables processing-structure-property relationships to guide the design of thinner yet stronger BVSs.
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