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Etude des interactions de surface et biocompatibilisation de nanocristaux fluorescents / Study of surface interactions and biocompatibilization of fluorescent nanocristalsKnittel, Fabien 11 October 2013 (has links)
Durant cette thèse nous avons, dans un premier temps, mis au point un protocole robuste pour quantifier l’échange de ligands à la surface de nano-objets, en prenant les quantum dots comme particules d’étude. Cette méthode se base sur la sensibilité de détection d’un élément radioactif, le tritium. Pour étudier l’échange de ligands, nous avons synthétisé de l’acide oléique tritié, dont l’équivalent non-marqué est un composé très couramment utilisé dans la chimie des QD. Nous avons élaboré un protocole permettant de déterminer la densité de ligands à la surface de quantum dots de type CdSe zinc blende par une méthode innovante. Par ailleurs, nous avons réalisé une étude permettant de déterminer la capacité qu’a un ligand à remplacer l’acide oléique présent à la surface des QD. On a ainsi obtenu une échelle des forces relatives de liaison de diverses fonctions chimiques suivant leur aptitude à déplacer l’acide oléique. Cette étude devrait permettre d’améliorer la compréhension et la mise au point des protocoles utilisés pour la préparation des QD. Dans un second temps, nous avons développé deux stratégies d’encapsulation de QD afin de les solubiliser dans l’eau avec comme objectif des applications en imagerie in vivo. Ces deux approches tentent de répondre aux nombreuses exigences liées à l’utilisation de QD en milieux biologiques. Dans cette optique, nous avons synthétisé des amphiphiles polymérisés d’une part et des amphiphiles perfluorés d’autre part. Des lots de QD, de type CdSe/CdS/ZnS émettant dans le visible, solubilisés selon ces deux stratégies ont été préparés et leur stabilité éprouvée dans plusieurs conditions. Nous avons ensuite appliqué l’encapsulation à des QD de type CuInS2/ZnS émettant dans le proche infrarouge. Des études préliminaire sont pu être réalisées par d’imagerie de fluorescence chez la souris afin d’évaluer in vivo ces nouvelles formulations de QD. / In this thesis we have, at first, developed a robust protocol to quantify the exchange of ligands on the surface of nano-objects, using quantum dots in this study. This method is based on the detection sensitivity of a radioactive element, tritium. To study the exchange of ligands, we synthesized tritiated oleic acid, whose unmarked equivalent is commonly used for the synthesis of QD. Thanks to an innovative method, we have developed a protocol to determine the density of ligands on the surface of zinc blende CdSe quantum dots. In addition, we conducted a study to determine the ability of a ligand to replace oleic acid on the surface of the QD. A scale of relative bond strengths of various chemical functions according to their ability to displace oleic acid has been obtained. This study is expected to improve the understanding and the development of protocols for the preparation of QD.In a second step, we developed two encapsulation strategies of QD in order to obtain colloidal stability in water with in vivo imaging applications as final aim. Both approaches attempt to answer the requirements for the use of QD in biological media. In this context, we have synthesized photopolymerisable amphiphilic compounds on the one hand and perfluorinated amphiphilic compounds on the other. Batches of CdSe/CdS/ZnS QD emitting in the visible, solubilized by these two strategies have been prepared and their stability tested in several conditions. We then applied the encapsulation strategy developed to CuInS2/ZnS QD emitting in the near infrared. Some preliminary studies have been carried out by in vivo fluorescence imaging in mice to assess these new QD formulations.
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A Response Surface Study of Extruded Corn Starch/Skim Milk Powder BlendsSingh, Sachin 01 May 1994 (has links)
Skim milk was ultrafiltered to three lactose/protein ratios and spray dried. The skim milk powder was extruded with pearled corn starch at different moisture contents, protein contents, lactose/protein ratios, and feed rates (control variables). Response surface methodology and a central composite in cube experimental design were used. This design required 30 experimental runs with 16 factorial points, 8 axial points, and 6 center points for replication. The physical and functional properties evaluated were expansion ratio, product temperature, bulk density, color, shear stress, viscosity, and water absorption index (response variables). Scanning electron microscopy was done to evaluate the microstructural attributes of the extrudates.
A quadratic model was used to express the response variables in terms of the control variables. Response surfaces were generated by assigning center point values to 2 of the 4 control variables and then solving the fitted equations as a quadratic in the remaining 2 control variables.
An increase in moisture content decreased expansion ratio, product temperature, color, and water absorption index, and increased bulk density, shear stress, and viscosity. An increase in protein content decreased product temperature, shear stress, viscosity, and water absorption index, increased color, and had no effect on expansion ratio and bulk density. An increase in lactose/protein ratio decreased product temperature, viscosity, and water absorption index, and had no effect on expansion ratio, bulk density, color, and shear stress. Feed rate did not have significant individual effect on any response variable. Expansion ratio had a negative correlation with bulk density (r = -0.61) and shear stress (r = -0.62) and a positive correlation with product temperature (r = 0.52). Bulk density and shear stress were positively correlated (r = 0.69), and product temperature and water absorption index were positively correlated too (r = 0.81). Expansion ratio, bulk density, color, and shear stress were chosen to determine a combined set of extrusion conditions most likely to produce an extrudate with properties suitable for a snack-type product.
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Characterization of epitaxial graphene grown on silicon carbide / Karaktärisering av epitaxiellt grafen växt på kiselkarbidJansson, Anton January 2014 (has links)
In this thesis work several manufacturing methods for graphene is discussed followed by an indepth study of graphene grown by a high temperature sublimation method (sublimation of siliconcarbide). The graphene surfaces studied have been grown by Graphensic AB, both graphenegrown on the Si-face and the C-face of the silicon carbide were studied. Six graphene samplesgrown 4H-SiC substrates were examined for homogeneity and surface morphology as well assome surface roughness parameters using Atomic Force Microscopy (AFM). The graphene wasstudied to get a better understanding of the surfaces and the growth mechanisms to improvemanufacturing parameters while also being informative for graphene sample customers. Anadditional graphene sample grown on 6H-SiC epitaxial layer was also studied to get a betterunderstanding of the sublimation mechanism. If graphene could be manufactured in a cheaprepeatable way the applications are endless and a new era of technology could emerge muchlike the silicon era that began several decades ago. In this thesis work the results are presentedas topography images as well as tables and histograms in the results section. The growth onthe Si-face is found to be well ordered when compared to the C-face which shows signs of alargely complex growth. The graphene on the Si-face lies on top of silicon carbide steps like acarpet with a buer layer interface against the silicon carbide. On the C-face this buer layeris not present but the graphene is deformed by buckling which is suspected to originate fromdierences in thermal properties between the graphene and the C-face. The in uence of AFMsettings for characterization of graphene while using intermittent mode have been evaluated andrecommendations are given. Finally a method for evaluating the homogeneity of the graphenelm is proposed but is in need of further verication.
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