Dissertations / Theses: 'SILICA SYSTEMS'

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Perry, Carole Celia. "Silicification in biological systems." Thesis, University of Oxford, 1985. http://ora.ox.ac.uk/objects/uuid:ae665ac4-63eb-4963-845a-d2db6aea31a6.

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This thesis is concerned with the formation and structure of silicified deposits in biology. The major system studied is silicified macrohairs from the lemma of the grass Phalaris canariensis L. The macrohairs consist of silica and polysaccharides. Chemical and structural studies on the mineral phase utilised electron microscopy (transmission (TEM), scanning (SEM) and ultra high resolution (HRTEM)), energy disoersive X-ray analysis (EDXA), solid state nuclear magnetic resonance ( ᷣ⁹ Si nmr), infrared spectroscopy, birefringence and nitrogen adsorption experiments. Results showed that the silica is chemically 'pure', hydrated, amorphous at a resolution of 1OÅ and a variety of structural morphologies were observed which are related to the maturity of the macrohair. Analytical studies at different times after emergence of the inflorescence utilising EDXA and scanning proton microprob eanalysis (SPM) showed that the inorganic elements Si, K, P, S and Cl are spatially organised within the macrohairs during silicification. It is proposed that the macrohairs are silicified under strict cellular control. The organic matrix in the mature macrohairs was investigated by acid hydrolysis and chromatography. The changing emphasis of polysaccharide synthesis in the macrohairs as mineralisation occurs was followed by in vivo radioactive labelling of inflorescences at different stages using ⁱ⁴C glucose and Harabinose. Analysis o fpolysaccharides synthesised involved acid hydrolysis and enzymic digestions (Amylase and Driselase), followed by paper and thin layer chromatography with scintillation counting of the products. Results showed that at the early stages of mineralisation, arabinoxylans and cellulose are the major polymers synthesised but as the macrohair matures, largely non-cellulosic glucans (as yet unidentified) are synthesised. It is proposed that the change in emphasis of polysaccharide synthesis during wall development is related to the size and ultrastructural arrangements of silica particles observed. The organic matrix was also observed to give additional order to the system, the resulting material being totally impervious. A second system, chosen for comparison, is mineralised teeth from the radula of the common limpet Patella vulgata. The mature teeth contain silica, iron oxide (goethite) and an organic matrix. Investigations on the silicified phase utilising electron microscopy revealed morphological structural variations. Analytical studies involving EDXA and SPM analysis showed that there are complex temporal and spatial variations in the inorganic composition (P, S, Ca, Fe, Si, Cu) in all regions of the teeth. It is proposed that these changes can be correlated with changes in composition of the organic matrix. A comparison is made of the silica from the two systems.

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Turner, Richard John. "The rheology and structure of aqueous gelatin-silica systems." Thesis, University of Bristol, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.274624.

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Kokhanenko, Pavlo. "Hydrodynamics and chemistry of silica scale formation in hydrogeothermal systems." Thesis, University of Canterbury. Mechanical Egineering, 2015. http://hdl.handle.net/10092/10247.

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The extraction of geothermal heat can cause precipitation of the minerals dissolved in geothermal fluid. Their deposition on the walls of wells and above-ground plant and in pores near reinjection wells, also known as mineral scaling, is one of the main obstacles to increasing the effectiveness of utilization of the limited geothermal resources. If not controlled properly it can result in accumulation of a significant amount of scale which obstructs pipes and reinjection wells and reduces the efficacy of heat exchangers. The most abundant mineral in geothermal fluid is silica and thus its precipitation can cause the highest scaling rate. While this dissertation is devoted to the study of silica scaling the results obtained may be applicable to other minerals with similar deposition mechanism. Oversaturated silica is known to precipitate from aqueous solution either by the direct chemisorption of single silicic acid molecules (monomers) or by forming colloidal particles suspended in the solution. These particles can subsequently be transported to, and attach onto, a wall. This process of colloidal silica deposition was previously recognised to cause much faster scaling than the direct deposition of silica monomers under typical geothermal plant conditions. While the chemical kinetics of silica polymerization and colloid formation are relatively well understood, transport of these colloids and their stability, which control their aggregation and attachment rates, on the other hand are not. Previous studies of the silica scaling process have identified prominent effects of geothermal brine hydrodynamics on the scaling rate. It was found to increase with the flow rate and particle size, thus suggesting the dominance of the advective (inertial) deposition of colloidal silica. However, this conclusion contradicted the present theory of particle transport in turbulent flows which argues the dominance of the diffusive transport for the relevant range of particle sizes (<1 μm). The development and continuing improvement of the anti-scaling measures required deeper understanding of the complex combination of the phenomena involved in the process of silica scaling. This was pursued in the present study using theoretical and experimental methods. First, the rate of colloidal silica transport from a turbulent flow onto the internal surface of a circular pipe, a cylinder and a flat plate were calculated using available analytical and numerical methods. The obtained theoretical transport rate was found to be about four orders of magnitude higher than the corresponding experimental scaling rate. The latter was determined in the previous studies to be 4.2·10-8 kg/s/m2 for silica colloids of 125 nm in diameter which corresponded to the dimensionless deposition velocity (the dimensionless deposition velocity is the scaling rate normalised by the particle mass concentration and friction velocity) of 1.2·10-6 for the dimensionless particle relaxation time of 2·10-4. Next, based on the standard DLVO theory of particle interactions and in the framework of the Smoluchowski approach the probability of colloidal silica particle attachment to a wall was found to be 10-6. Therefore, the theoretical scaling rate, calculated as a product of this probability and the above-mentioned transport rate was two orders of magnitude lower than the experimental scaling rate. This suggested that the implemented theoretical approach either underestimated particle transport rate or overestimated particle stability. Both possibilities are explored in this dissertation. In addition, the silica scaling rate was measured for a range of conditions: particle size from 20 to 60 nm, particle concentration 1600-10000 ppm, friction velocity from 0.09 to 0.18 m/s (Re = 9-50·103) and ionic strength from 30 to 80 mM, pH 8.1-9.5 and temperature from 25 to 44 °C. For this, laboratory experiments were designed and progressively modified in order to improve the repeatability of the results and to study the scaling process. In these experiments colloidal silica deposition onto the walls of mild steel pipe sections was studied with a recirculating flow rig with variable (but controllable) particle size, concentration, flow rate, pH and ionic strength of the solution. In addition, a parallel plate flow test section was designed and built which will provide better capabilities for the control over the hydrodynamic and test surface conditions in future experiments. The control over the chemical conditions was achieved by the use of the synthetic colloidal solutions. Two methods of their production – hydrolysis of either sodium metasilicate or active silicic acid – were employed. The influence of the synthesis conditions, ion content and pH on the long term behaviour of these colloidal solutions was investigated. The particle size data, obtained using dynamic light scattering (DLS) and verified by electron microscopy, was analysed and compared against the predictions of the current models of nanoparticle growth and stability. The kinetic aggregation was identified to be the dominant particle growth mechanism. Experimental data collected during the long-term observations of the particle growth allowed relationships between the aggregative stability and such parameters as the particle size, ion concentration and pH of the solution to be elucidated. In particular, the aggregative stability of 10-20 nm particles was found to be 108-1010 which is 7-9 orders of magnitude higher than the corresponding DLVO stability. It was also found to decrease with the increase of the particle size. This agreed with the theory of the colloid stabilization by steric interactions. Moreover, the model of the “gel” layer was used to explain the observed “anomalies” of the colloidal silica behaviour. The deposition experiments conducted with these synthetic colloidal solutions showed that the scaling rate increased with the particle size, flow rate and ionic strength (IS) of the solution. Thus, it was measured to be 9.7·10-9 kg/s/m2 for the 45 nm particles in a solution with IS = 0.05 M, which corresponded to the dimensionless deposition velocity of 6.6·10-8 for a dimensionless particle relaxation time of 2.2·10-6. The scaling rate was calculated for these conditions by multiplying the corresponding transport rate and the actual attachment probability determined as an inverse of the experimental stability. It was found to agree with the experimental value within an order of magnitude. In addition, the observed increase of the scaling rate with the increase of particle size was explained by the compensation of the decreased rate of the particle transport by faster decrease of actual particle stability (increase in attachment probability). Therefore the contradiction between the theory and the experiment was resolved for the particles of 20 to 60 nm in diameter. Moreover, the observations of the dimensions and distribution of the scale elements formed in some of the present experiments strongly suggested the significance of the advective (inertial) mechanism of particle deposition. This and comparative analysis of other experimental and theoretical data suggested that the present theory may underestimate the convective transport of the particles onto a rough wall. Therefore, the hypothesis of the parallel-to-wall advective deposition of the nanoparticles onto the roughness/scale elements (not accounted in the current theory) was proposed. The corresponding mass transfer problem was solved analytically using experimentally found dimensions of the scale elements. The additional transport was found to decrease the above-stated discrepancy between the theoretical and experimental scaling rate for large (125 nm) particles by one order of magnitude. The remaining difference of one order of magnitude was speculated to be due to the underestimation of these particles attachment probability derived with the standard DLVO theory. The actual aggregative stability of the silica colloids larger than 60 nm in diameter and for a wider range of IS values is of interest for future experimental studies. An improved understanding of the interrelation between the chemical and hydrodynamic phenomena in the process of silica scaling and its dominant mechanisms was achieved in this dissertation. This allowed optimization of the present anti-scaling practices aimed to minimize the negative effects of mineral scaling on the operation of geothermal power stations. Besides the practical recommendations, which may ultimately help to increase the efficiency of geothermal power stations, the results of the present study may be of value in the fields of mass transfer and colloid science.

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Rashchi, Fereshteh. "Adsorption on silica in Pb- and Ca-SO4-CO3 systems." Thesis, McGill University, 1996. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=27252.

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Formation of Pb and Ca precipitates on a silica surface in the presence of sulphate and carbonate under neutral to alkaline condition is studied using zeta potential measurements, Scanning Electron Microscopy (SEM), and X-Ray Photoelectron Spectroscopy (XPS). The effect of carbonate on displacing sulphate is discussed.
In the Pb/sulphate system, precipitates of predominantly Pb-oxide/hydroxide formed on the silica surface. In the Pb/carbonate system, the precipitates were predominantly Pb-carbonate/hydroxy carbonate. Precipitates in both the Pb/SO$ sb4$ and Pb/CO$ sb3$ systems were dispersed by addition of sufficient carbonate, the silica surface eventually becoming free of precipitates. This dispersion was considered to be due to: a high negative surface charge density on both lead carbonate and silica; nucleation being promoted at high concentrations of carbonate, resulting in small precipitates; and increased solubility at high carbonate concentrations.
In the Ca system, calcium sulphate precipitates did not form on the silica particles while calcium carbonate precipitates did. The precipitates were not removed by increasing carbonate concentration. The difference from the Pb system is attributed to a low negative surface charge density on calcium carbonate compared to lead carbonate, leading to less dispersing conditions, and the higher solubility of calcium sulphate compared to lead sulphate.

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Meadows, Philippa Jill. "Template-directed synthesis of silica materials based on self-assembling systems." Thesis, University of Bristol, 2006. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.439957.

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Rezk, Ahmed Rezk Masoud. "Theoretical and experimental investigation of silica gel/water adsorption refrigeration systems." Thesis, University of Birmingham, 2012. http://etheses.bham.ac.uk//id/eprint/3623/.

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This PhD project was set out to improve the performance of silica gel / water adsorption cooling systems using a number of investigation tools. A novel global lumped analytical simulation model has been constructed for a commercialised two-bed silica gel / water 450kW adsorption chiller. It was integrated with a genetic algorithm (GA) optimisation toolbox to determine the optimum operating conditions to obtain the optimum chiller performance. The model was used to investigate the effect of physical and operating on the chiller performance. The model was also used to investigate the effect of various adsorbent bed enhancement techniques that are presented in published literature. An experimental test facility has been designed, constructed and commissioned to study the performance of scaled down adsorbent bed modules. It has been constructed to understand the effect of the operating conditions on adsorbent-bed heat and mass transfer performance. A dynamic vapour sorption (DVS) gravimetric analyser has been used to characterise a new species of adsorbents (MOFs). These adsorbents have strong potential towards water sorption and could replace the currently applied silica gel. MOFs adsorbents have been characterised in terms of adsorption isotherms and kinetics, in addition to its cyclic analysis. It was found that HKUST-1 (copper based MOF) outperforms silica gel with 95.7% increase in the water uptake. Iron based MOF (MIL-100) was found to outperform silica gel for high evaporating temperature application.

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Neugebauer, Adam (Adam Halbert). "Thermal properties of granular silica aerogel for high-performance insulation systems." Thesis, Massachusetts Institute of Technology, 2013. http://hdl.handle.net/1721.1/85213.

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Thesis: S.M. in Building Technology, Massachusetts Institute of Technology, Department of Architecture, 2013.
This electronic version was submitted by the student author. The certified thesis is available in the Institute Archives and Special Collections.
Cataloged from student-submitted PDF version of thesis.
Includes bibliographical references (pages 65-67).
Based on mounting evidence in support of anthropogenic global climate change, there is an urgency for developments in high-performance building techniques and technologies. New construction projects provide substantial opportunities for energy efficiency measures, but they represent only a small portion of the building stock. Conversely, while existing buildings are plentiful, they typically have a much narrower range of feasible energy efficiency options. Therefore, there will continue to be a need for the development of new and improved energy efficiency measures for new building construction and even more so for deep retrofits of existing buildings. This thesis provides an overview of the research performed into the on-going development at MIT of a high-performance panelized insulation system based on silica aerogel. Two test methods were used for measuring the thermal conductivity of the granules: the transient hot-wire technique and the guarded hot-plate system. Utilizing the hot-wire set-up, it was demonstrated that compressing a bed of granules will decrease the thermal conductivity of the system until a minimum point is reached around the monolithic density of the aerogel. For the Cabot granules, this was seen at 13 mW/m-K and about 150 kg/m3. The MIT granules showed equal performance to the Cabot granules at bed densities 20-30 kg/m3 lower. The hot-plate testing was able to experimentally evaluate previous analytical predictions regarding the conductivity impact of the internal panel truss and the under-prediction of radiant heat transfer in the hot-wire method. Hot-wire testing was also done in a vacuum chamber to quantify potential performance improvements at reduced air pressures. Since a vacuum would require the incorporation of a barrier film into the panel system, some analyses were done into the thermal bridging potential and gas diffusion requirements of such a film. Additionally, physical prototyping was done to explore how the film would be incorporated into the existing panel design. The aerogel-based insulation panel being developed at MIT continues to show promise, though there are still plenty of opportunities remaining in the development cycle.
by Adam Neugebauer.
S.M. in Building Technology

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Huang, Pengyu. "Multiscale Modelling of Dynamic Contact Angles for CO2-Water-Silica Systems." Thesis, The University of Sydney, 2019. http://hdl.handle.net/2123/20937.

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The capillary and dynamic wetting behaviour in porous media is crucial in many engineering problems which are highly related to the multiphase interactions between fluids and solids. This thesis will focus on the behaviour of dynamic contact angle of the supercritical CO2/water flow in the silica slit as a function of the contact line velocity at both the nanoscale and microscale, which can help us gain an in-depth understanding of the dynamic processes in CO2 geosequestration in saline aquifers. Our molecular dynamics (MD) simulations calculate the contact angle quantitatively at different velocities at the nanoscale and also validate the molecular kinetic theory through the detailed analysis of the equilibrium jump distance and frequency of the water and CO2 molecules at the solid surfaces. While the MD simulations provide the results of dynamic contact angle at the nanoscale, which can be suitable for the nanopores of the low permeability rock, the dynamic contact angle behaviour at the microscale is also important and investigated in this thesis. This work also develops a coarse-grained molecular dynamic (CGMD) framework to model the liquid-vapour-solid interactions at the microscale. The newly developed CGMD framework has been applied and extended to the study of the dynamic contact angle for the CO2-water-silica system at the microscale. The microscale CGMD simulation of CO2-water-silica system shows that there is an increase in the CO2 contact angle as the increase of the contact line velocity at three different pressures. The dynamic contact angles under a water pressure of 18.9 MPa seem to be slightly larger than those under the water pressures of 9.41 MPa and 14.3 MPa. Moreover, the comparison between the MD and CGMD results suggests that there could be a pore size effect on the dynamic contact angle for the studied CO2-water-silica system.

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NAIRI, VALENTINA. "Functional ordered mesoporous silica in nanomedicine: target and drug delivery systems." Doctoral thesis, Università degli Studi di Cagliari, 2018. http://hdl.handle.net/11584/255981.

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Ordered mesoporous materials (OMMs) are characterized by high surface area (up to 1000 m2/g), high pore volume (1-3 cm3/g) and narrow pore size (2-30 nm) distribution. Recently, mesoporous silica nanoparticles (MSNs), a subclass of OMMs, have had great development as nanocarriers for drug delivery, particularly for cancer treatment. The research activity of my PhD work was aimed to study SBA-15 and MCM-41 mesoporous silica samples for biomedical applications. The texture and the structure of the synthesized materials were characterized through N2 adsorption/desorption isotherms, SAXS, and TEM. The functionalization of the mesoporous silica samples was verified by means of Fourier-transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). DLS and ELS were used to determinate hydrodynamic diameter and zeta potential of the studied systems under different conditions. The PhD thesis focused on different aspects of the use of OMMs, particularly MSNs, as drug nanocarriers. In the first paper how different features of OMMs (surface area, pore size and surface charge) can affect the adsorption and release of drugs was investigated. Ampicillin, a penicillin-like -lactam antibiotic was loaded on MCM-41, SBA-15, and amino-functionalized SBA-15, then its release in simulated physiological conditions was studied. This study demonstrated that to obtain a sustained drug release, the chemical nature of the matrix’s surface plays a role which is more important than its textural features. SBA-15-NH2 matrix is a suitable candidate as depot system for local sustained release of ampicillin. Common target systems have the disadvantage that the targeting molecule can be recognized by several receptors. A possible strategy to solve this issue was investigated in the second paper. The targeting molecule was hidden by preparing a double sequential targeting system. To this purpose a double target system was synthesized. Alendronate was used as a tissue target to recognize a diseased bone, and an encrypted cellular target, Arg-Gly-Asp (RGD) was used to improve the internalization in human osteosarcoma cells (collaboration with Universidad Complutense de Madrid). This preliminary study showed the efficacy of the double target systems. The next step could be the functionalization of MSNs with the previously described systems for the synthesis of a smart target systems usable as a carrier for anticancer drugs against bone cancer. In the third paper, the effect of surface charge on the internalization of MCM-41-type MSNs, functionalized with chitosan (CHIT) and hyaluronic acid (HA) biopolymers, on 3T3 mouse fibroblast cells was then investigated. The opposite surface charge of the biopolymer-functionalized MSNs (negative for MSN-HA and positive for MSN-CHIT) gave a different interaction with BSA, used as a model protein to investigate the formation of the protein corona (forth paper). Finally, in the fifth paper, MSNs were functionalized with HA samples having three different molecular weights (HAS, HAM, and HAL). The effect of HA molecular weight on the internalization of HA-MSNs particles on HeLa cells was evaluated. These last studies showed the importance of the external functionalization on the interaction between MSNs and the components of body fluids, that change their surface properties. These changes as well as the polymer’s features (i.e. the molecular weight) are able to modulate the cellular uptake. The obtained results highlight the importance of the physico-chemical phenomena occurring at the nano-biointerface for the future use of functionalized OMMs and MSNs in nanomedicine. The present findings confirm that these nanocarriers are very promising matrices for the obtainment of targeting drug delivery systems for cancer treatment.

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Rahman, Shaily. "Cosmogenic Silicon-32 reveals extensive authigenic clay formation in deltaic systems and constrains the marine silica budget." Thesis, State University of New York at Stony Brook, 2016. http://pqdtopen.proquest.com/#viewpdf?dispub=10140185.

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Cosmogenic ³²Si (t_1/2 ∼ 140 yrs) was used in a novel way to constrain the quantity of reactive Si storage and early diagenetic reactions of Si in the highly mobile deltaic sediments along the coast of French Guiana, representative of deposits along the ~1600 km Amazon–Guianas coastline downdrift of the Amazon delta. A sequential leach was developed to extract and purify SiO₂ from different operational pools in large samples of surface sediments (0–10cm). This methodology, a hot 1% Na₂CO₃ leach followed by a hot 4M NaOH leach, was adapted from the existing leaches widely used to estimate biogenic silica (bSi) content in marine sediments, and ultimately to constrain the global oceanic Si budget. ³²Si activity was determined in each pool via its daughter product ³²P. Results from several sites in coastal mudbanks near Kourou and Sinnamary indicate no detectable ³²Si activity in the bSi fraction, whereas ³²Si was detected in the Si-NaOH fraction after removal of bSi. The lack of detectable activity in the 1% Na₂CO₃ leach and its detection in the NaOH fraction (0.4–2.5 dpm) indicate that the method widely used to determine bSi content recovers only a minor fraction of the originally deposited reactive bSi in these deposits. The results are consistent with rapid alteration of biogenic silica and clay authigenesis or reverse weathering. They also demonstrate that the current estimate of biogenic silica storage in tropical deltaic sediments is significantly underestimated. Assuming an initial diatom specific activity range of ∼5–40 dpm/kg SiO₂, the ³²Si activity in the NaOH fraction corresponds to a reactive Si storage of ∼150–18,000 µmol Si/g sediment. This magnitude is more consistent with estimates of reactive Si (ΣSi_hr) storage in the Amazon delta based on modified operational leach techniques that target poorly crystalline clays and with diagenetic modeling of pore water K⁺, F⁻, and Si(OH)₄, though these modified leaches also appear to underestimate the amount of reactive Si stored along this system. To directly confirm whether these modified operational extractions underestimate reactive Si storage, a sequential extraction methodology was also developed to first isolate ³²Si activity in the ΣSi_hr fraction (0.1N HCl followed by 1% Na₂CO₃) and then extract any remaining ³²Si from the residual fraction using 4M NaOH.

Sediment from 2 stations in the Gulf of Papua, Papua New Guinea, 1 station in the northern Gulf of Mexico near the Southwest Pass, and 1 station in Long Island Sound (Smithtown Bay) were also extracted for ³²Si in the bSi fraction as well as the residual fraction after removal of bSi. Bulk ³²Si activities in the residual fractions in the Gulf of Papua (0.5–0.7 dpm/kg sediment) were used to extrapolate Si storage in the outer topset and forset of the clinoform delta.

³²Si activity was detected in the both the bSi (0.21 ± 0.04 dpm/kg sediment) and the residual fraction (0.44 ± 0.08 dpm/kg sediment) from the site in the Gulf of Mexico. A Si burial rate using the ³²Si activity in the bSi fraction (assuming an activity of 15dpm/kg in starting Si materials) of 0.004Tmol/y was calculated over approximately 5000 km2 of the delta, whereas the burial rate calculated using the Si content in this same fraction from a classic bSi leach, was ∼0.006Tmol/y. Adding the Si burial rate using the ³²Si activity in the residual fraction (0.008Tmol/y) yielded a total storage per year of 0.012Tmol Si, ∼10% of the total Si inputs (dissolved and amorphous Si) from the Mississippi-Atchafalaya river system. ³²Si activity was also detected in the residual fraction (0.53 ± 0.08 dpm/kg sediment) after removal of ΣSi_hr and using this activity yielded similar calculated rates of Si burial (∼0.01 Tmol/y).

In Smithtown Bay, Long Island Sound, ³²Si activity was also detected in both the bSi (0.15 ± 0.05 dpm/kg sediment) and the residual (0.4 ± 0.2 dpm/kg sediment) fractions from the site in Smithtown Bay, Long Island Sound, yielding a total Si storage estimate (assuming an activity of 15 dpm/kg in starting Si materials) of 1.6 × 10⁻³ Tmol/y over the entire Sound, comparable to estimates of Si storage calculated using the Si content in the classic bSi (1.1 × 10⁻³ Tmol/y) and the classic ΣSi_hr (2.2 × 10⁻³ Tmol/y) leaches. It appears that reverse weathering is an important sink of Si in these deposits and that classic bSi or ΣSi_hr leaches can underestimate Si storage in these system by two to four-fold. (Abstract shortened by UMI.)

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Cervantes, Martínez Claudia Violeta. "Porous and hybrid silica from biocompatible systems : application to drug release." Electronic Thesis or Diss., Université de Lorraine, 2019. http://www.theses.fr/2019LORR0295.

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L'objectif de ce travail se concentre sur la préparation de matériaux poreux silicatés hybrides et dopés avec un principe actif, à base de composants biocompatibles pour des applications pharmaceutiques, en tant que systèmes d’administration de médicaments. La motivation de cette étude est liée à la nécessité de répondre à la demande croissante de médicaments plus efficaces. Le premier point d'intérêt de cette étude concerne les composés utilisés qui sont biocompatibles, peu coûteux, et qui, sont de bons candidats pour la formation de matériaux mésostructurés. Le tensioactif utilisé était le Kolliphor EL (KEL) et les huiles retenues étaient le Miglyol 812N (Mig), et le Myristate d’Isopropyl (IM). Le principe actif le Kétoprofène (KTP) a été choisi comme molécule modèle pour l’évaluation de les essaies de libération. En fin, les cellules HeLa, un type particulier de cellules cancéreuses, ont été utilisées pour évaluer la toxicité des matériaux synthétisés. Le premier chapitre est consacré à l'état de l'art des structures moléculaires à partir des tensioactifs non-ioniques, en particulière le KEL. Ensuite, les principales publications relatives aux matériaux poreux et hybrides en tant que vecteurs de drogues sont résumées. À la fin de ce chapitre, les modèles cinétiques de libération et les équations correspondantes sont présentées. Le second chapitre rassemble les modes opératoires et les techniques de caractérisation utilisés Le troisième chapitre étude le comportement de phase du système binaire KEL/eau étudié dans le cadre de ce travail est décrit. Les différents domaines à 1 et 2 phases ont été déterminés et caractérisés par inspection visuel, à l’aide de la microscopie optique à lumière polarisée et les structures aux des cristaux liquides par SAXS. Ensuite, l'influence de l'addition d’huile dans le système KEL/eau a été étudié à 25 °C Les diagrammes de phase ternaire ont été établis avec Miglyol (Mig) et Isopropyl Myristate (IM). À partir de ces systèmes à base de Mig et IM, des matériaux mésoporeux ont été préparés. Avec des conditions de synthèse optimisées, on a réussi à structurer le réseau mésoporeux dans les deux cas. Dans le quatrième chapitre l’influence de l’addition d’un copolymère block, le P123 dans le système KEL/eau est reportée et le diagramme de phase est présente. Il a permis d'évaluer la synergie des deux tensioactifs pour former des micelles et des cristaux liquides. Ensuite, l’effet de l’addition de micelles de P123 dans les émulsions fines á base d’Isopropyl Myristate sur les caractéristiques des matériaux poreux ainsi préparés en utilisant différentes teneurs de micelles de P123, il est possible de faire varier le degré de porosité des matériaux. Pour des proportions émulsions (Em)/micelles P123 inférieures à 50/50, on obtient des silices mésoporeuses avec deux tailles de pores. Lorsque le rapport Em/P123 augmente, est possible de contrôler la porosité des matériaux. Le cinquième chapitre concerne sur l'étude de l'encapsulation de KTP dans différents systèmes et de sa libération. Des émulsions concentrées ainsi que des matériaux hybrides à base de solutions micellaires et d'émulsions fines ont été sélectionnés. Les études de libération ont été effectuées avec une solution de PbS a différents pH :7,4; 1,2 et 4,6. Les résultats ont montré que, dans des conditions neutres, le KTP libéré par les matériaux hybrides à base des solutions micellaires atteint 38% au bout de 24h et l’effet du pH permet d’augmenter la quantité de KTP libéré. Ensuite, la libération dans une solution réceptrice avec diffèrent concentrations de P123 a été étudié. Les résultats montrent que la quantité de KTP libéré en présence de 5% de P123, atteindre 65% au bout de 24h. Dans la dernière partie, la toxicité des matériaux et des systèmes hybrides dopés a été évalué. Les résultats montrent que la matrice de silice protège les cellules car la viabilité cellulaire est augmentée, de 64 à presque 80% avec les matériaux hybrides
The objective of this work focuses on the preparation of porous, hybrid silicate materials doped with an active ingredient, based on biocompatible components for pharmaceutical applications, as drug delivery systems. The motivation for this study is related to the need to meet the growing demand for more effective drugs. The first point of interest of this study concerns the compounds used which are biocompatible, low-cost, and which are good candidates for the formation of mesostructured materials. The surfactant used was Kolliphor EL (KEL) and the oils were Miglyol 812N (Mig), and Isopropyl Myristate (IM). The active ingredient Ketoprofen (KTP) was chosen as the molecule model for the evaluation of release assays. Finally, HeLa cells, a cancer cell, were used to assess the toxicity of the synthesized materials. The first chapter is devoted to the state of the art of molecular structures based on non-ionic surfactants as KEL. Then, the main publications relating to porous and hybrid materials as drug carriers are summarized. At the end of this chapter, the kinetic release models and corresponding equations are presented. The second chapter brings together the methods and characterization techniques used. The third chapter studies the phase behaviour of the KEL/water binary system studied in this work and is described. The different 1- and 2-phase domains were determined and characterized by visual inspection, using polarized light optical microscopy and liquid crystal structures by SAXS. Then, the influence of oil addition in the KEL/water system was studied at 25°C. Ternary phase diagrams were established with Miglyol (Mig) and Isopropyl Myristate (IM). From these Mig and IM-based systems, mesoporous materials were prepared. With optimized synthesis conditions, the mesoporous network was structured in both cases. In the fourth chapter the influence of the addition of a block copolymer, the P123 in the KEL/water system is reported and the phase diagram is present. It evaluated the synergy of the two surfactants to form micelles and liquid crystals. Then, the effect of the addition of P123 micelles in Isopropyl Myristate based fine emulsions on the characteristics of the porous materials thus prepared using different P123 micelle contents, it is possible to vary the degree of porosity of the materials. For emulsion (Em)/micelle P123 proportions less than 50/50, mesoporous silicas with two pore sizes are obtained. When the Em/P123 ratio increases, it is possible to control the porosity of the materials. The fifth chapter concerns the study of the encapsulation of KTP in different systems and its release. Concentrated emulsions as well as hybrid materials based on micellar solutions and fine emulsions have been selected. Release studies were performed with a PbS solution at different pH levels: 7.4; 1.2 and 4.6. The results showed that, under neutral conditions, the KTP released by hybrid materials based on micellar solutions reaches 38% after 24 hours and the pH effect increases the amount of KTP released. Then, the release into a receptor solution with different concentrations of P123 was studied. The results show that the amount of KTP released in the presence of 5% P123, reach 65% after 24 hours. In the last part, the toxicity of doped materials and hybrid systems was assessed. The results show that the silica matrix protects the cells because cell viability is increased, from 64 to almost 80% with hybrid materials

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Rashchi, Fereshteh. "Adsorption on silica in Pb- and Ca-SO¦4-CO¦3 systems." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1997. http://www.collectionscanada.ca/obj/s4/f2/dsk2/ftp01/MQ29625.pdf.

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Wiputri, Yonika. "Microparticle retention aid systems in mechanical pulp suspensions." Thesis, University of British Columbia, 2008. http://hdl.handle.net/2429/973.

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In this thesis, the effectiveness of microparticle retention aid systems comprising of different cationic starches (tapioca and waxy maize), cationic flocculants (flocculant 1, linear with low charge density and flocculant 2, branched with medium charge density polyacrylamides) and anionic colloidal silica in improving retention and drainage of thermomechanical pulp (TMP) suspensions loaded with precipitated calcium carbonate (PCC) is studied. While starch is primarily added as dry strength agent in PCC-filled TMP suspensions, it also has a significant role in improving retention and drainage. Tapioca starch, which has both amylose and amylopectin, is found to be a better retention and drainage aid than waxy maize starch, which only contains amylopectin. In the absence of starch, both flocculants are ineffective in improving retention and drainage. With starch, both flocculant and silica are significant in enhancing retention and drainage further. Increasing the dosage of either flocculant or silica generally increases retention as well as drainage. Flocculant 2 is found to give slightly worse total and filler retention but better drainage compared to flocculant 1. The dosage of flocculant 2 is only half that of flocculant 1 though – for this reason overall flocculant 2 is deemed more effective in improving retention and drainage than flocculant 1. Split starch addition, where a portion of the starch is premixed with PCC and the rest added to the pulp, causes a slight decrease in both retention and drainage. Therefore, should the papermaker decide to use this approach, the starch should be split in a 25:75 ratio between PCC and the pulp to minimize the negative effects. Due to the cost benefits of using increased amounts of PCC, it is desirable to increase PCC content beyond the standard currently used (250 kg/t OD pulp for communications-grade paper). However, at very high dosages of PCC (500 kg/t OD pulp), the best combination identified in this work (tapioca starch, flocculant 2 and silica) is unable to maintain good retention and drainage. Increasing retention aid dosages may help retain more PCC, however this tactic can rapidly become uneconomical. A new approach is thus needed to achieve such highly-filled papers.

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Giri, Supratim. "Mesoporous silica nanomaterials and magnetic nanoparticles based stimuli-responsive controlled-release delivery systems." [Ames, Iowa : Iowa State University], 2008.

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15

Kupferschmidt, Natalia. "Toxicological and Immunomodulatory Properties of Mesoporous Silica Particles : Applications in Life Sciences." Doctoral thesis, Uppsala universitet, Nanoteknologi och funktionella material, 2013. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-195904.

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Mesoporous silica particles offer great potential benefits as vehicles for drug delivery and in other biomedical applications. They present a high loading capacity due their ordered and size-tuneable pores that allow molecules to be loaded and released. In addition, they offer the possibility to enhance oral bioavailability of drugs with limited aqueous solubility and to protect pH sensitive drugs from the acidic conditions in the stomach on their way to the intestine. The aim of this thesis was to evaluate the biocompatibility and effects of mesoporous silica particles on immunocompetent cells. Subsequently, two potential life sciences applications were investigated: as adjuvants and as weight reduction agents. Adjuvants are used in vaccines in order to enhance the immunological response towards attenuated and poorly immunogenic antigens. Their function can be mediated through dendritic cells which have a central role in the control of adaptive immunity including immunological memory. Our results show that different types of mesoporous silica particles were able to tune the development of T cells both in human cell cultures and in mice. In contrast to the approved adjuvant alum (aluminium salts) which is a specific inducer of Th2-type immune responses, the particles induced more Th1-like responses, which may be desired in vaccines against allergy and intracellular pathogens such as viruses. Particle exposure to macrophages did not affect their cell function which is crucial for tissue homeostasis, wound repair and in prevention of autoimmune responses. Likewise, the cytokine secretion was not affected, which suggest that macrophages would not modulate the immune response towards the particles. Furthermore, mesoporous silica particles were highly tolerated at daily oral administrations of up to 2000 mg/kg doses for some of the materials prepared. Large pore mesoporous silica particles were shown to act as weight and body fat reduction agents without other observable pathological signs when administered in the diet of obese mice. Together; those results are promising for the development of mesoporous silica as drug delivery systems and adjuvants for oral administration of drugs or vaccines. Additionally, large pore mesoporous silica materials are potential agents for the treatment of obesity.

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Davis, Jason Edward. "Geochemcial Controls on Arsenic and Phosphorus in Natural and Engineered Systems." Thesis, Virginia Tech, 2000. http://hdl.handle.net/10919/31012.

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This thesis elucidates fundamental reactions that can control concentrations of arsenic and phosphate in water sources. High levels of arsenic or phosphorus have significant implications for the environment-- arsenic is extremely toxic to humans while phosphorus can cause eutrophication. Initial work focused on arsenic solids that might exert geochemical control on soluble arsenic. Formation of proposed iron, barium, copper and zinc-arsenic solids were systematically examined under realistic environmental conditions. Thermodynamically favored copper, ferrous and barium solids did not form under circumstances of significance to drinking water sources. However, sorption of arsenic to iron, zinc and copper solids was discovered to be very significant, depending on the pH and solids age. Given the established importance of sorption in arsenic and phosphate chemistry, two key constituents (silica and sulfide) implicated in mobilization of sorbed arsenic or phosphate were examined in detail. The addition of silica, which competes with arsenate or phosphate for sorption sites on Al(OH)3 and Fe(OH)3 hydroxides, caused release of 0-30% sorbed As and P at pHs between 7.0 and 8.5. Reaction of sulfide with Fe(OH)3 led to instantaneous release of 50-95% of sorbed As and P through a reductive dissolution mechanism. This instantaneous release was slowly reversed as orpiment (As2S3) and vivianite [Fe3(PO4)2] slowly precipitated, but under other circumstances, these solids would not be expected to form. Modeling results suggest that arsenic and phosphate concentrations could either increase or decrease in response to reaction between Fe(OH)3 and sulfides, thereby reconciling literature reports that seemed to contradict one another.
Master of Science

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Khan, Jafar Iqbal. "Physics of colloid vibration potential for imaging ionic species and silica dioxide nanoparticle systems." Thesis, University of Leeds, 2010. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.531618.

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Han, Bing. "Prevention of Cathodic Delamination of Polyurethane from Titanium by Plasma Polymerized Silica/Aminosilane Primer Systems." University of Cincinnati / OhioLINK, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1491558395253426.

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Du, Na. "Investigation of Hydrogenated and Fluorinated Surfactant Based-Systems for the Design of Porous Silica Materials." Thesis, Nancy 1, 2010. http://www.theses.fr/2010NAN10046/document.

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Ce travail est consacré à l’étude des propriétés de systèmes à base de tensioactifs non ioniques hydrogéné et fluoré dans le but de préparer des matériaux poreux silicatés. L’effet de la solubilisation d’hexadécane ou de décane dans des micelles de C12H25CO(OC2H4)9OCH3 conduit à la formation de silices mésoporeuses à plus larges pores, tandis qu’aucun effet de gonflement n’est observé avec l’ajout de cyclohexane. Lorsque les matériaux sont préparés avec des micelles de C8F17C2H4(OC2H4)9OH, l’ajout de perflorooctylbromure (PFOBr) augmente la taille des mésopores. Par ailleurs, l’incorporation de grandes quantités de PFOBr ou de perfluorodécaline conduit à la formation de macropores. Avec C7F15C2H4(OC2H4)8OH, l’incorporation de (C4F9CH)2 permet d’élargir les mésopores et de créer un réseau de macropores, tandis que l’ajout de PFOBr ne conduit ni à la formation de mésopore, ni à la formation de macropore. Les résultats mettent en évidence que la formation de matériaux macroporeux à partir d’émulsions hydrogénées ou fluorées est favorisée avec les systèmes qui présentent des valeurs de PIT (Température d’Inversion de Phase) élevées. Pour finir, l’effet de l’addition de différents alcools dans le système à base de C8F17C2H4(OC2H4)9OH a été étudié. La détermination des paramètres structuraux de la phase cristal liquide hexagonal, indique que les alcools à courte ou moyenne chaîne jouent le rôle de solvant, tandis que le fluoro-octanol joue celui d’un co-tensioactif. L’addition d’alcools courts provoque la destruction progressive des micelles qui perturbe le mécanisme d’auto-assemblage et les matériaux obtenus présentent des structures vermiformes
This work deals with the study of the properties of nonionic hydrogenated and fluorinated surfactant based systems which are related to the synthesis of porous silica. The effect of the solubilization of low fraction of hexadecane or decane in the micelles of C12H25CO(OC2H4)9OCH3 leads to the formation of large mesoporous silica, whereas no swelling effect was noted with cyclohexane. When the materials are templated by fluorinated micelles of C8F17C2H4(OC2H4)9OH, large pore mesoporous materials are obtained with perfluorooctyl bromide (PFOBr). Both PFOBr and perfluorodecalin give rise to macropores at high oil concentrations. With C7F15C2H4(OC2H4)8OH, the fluorocarbon (C4F9CH)2 is not only an effective expander to enlarge the pore size of mesoporous materials, but also very favourable for the design of macropore network. On the contrary, with PFOBr, there is neither mesopore nor macropore. Therefore, both hydrogenated and fluorinated systems obey to the same rule: the formation of macroporous materials template by emulsions is favoured with systems which exhibit a high value of the PIT. Lastly, alcohols used as additives in the C8F17C2H4(OC2H4)9OH -water system to tune the characteristics of the recovered materials. The structural parameters of the hexagonal liquid crystal show the short and medium alcohols behaved like solvent, while the long chain and fluorinated octanol acted as co-surfactant. The short alcohols provoke a micelle breaking effect. Thus, the self-assembly mechanism is disturbed and wormhole-like structures are recovered

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Walker, Richard John. "Behaviour of nanocolloidal particles on mica : investigations using atomic force microscopy." Thesis, University of Edinburgh, 2010. http://hdl.handle.net/1842/4633.

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In this thesis we used atomic force microscopy (AFM) to investigate systematically the behaviour of both electrostatically stabilised silica and sterically stabilised polystyrene (PS) colloidal systems on freshly cleaved mica substrates. For the silica colloidal nanoparticles we explored the effect of colloidal suspension concentration, particle size, and different application techniques on both the adsorption behaviour and subsequent structuring of the particles. For the PS colloidal nanoparticles we explored concentration effects and experimented with both dip-coating and droplet application techniques. We showed that silica nanoparticles adsorbed onto mica via irreversible adsorption that possessed lateral mobility due to the weak attraction between the nanoparticles and the substrate, facilitating subsequent capillary structuring of the nanoparticles during drying. We associated the effects of volume fraction with Debye screening, and kinetics effects with particle size and volume fraction. We also successfully imaged a partially dried film and showed the role of convective/capillary forces in the structuring of the nanoparticles. Studies with variations in particle size generated a number of different topography structures; with dewetting phenomena observed for 10 nm nanoparticles and the formation of crystalline structures for 100 nm nanoparticles. Spin coating techniques were used to produce even larger crystalline structures of nanoparticles. Size dependent ordering occurred for low concentration samples due to the polydispersity of the colloidal suspension. We showed that acceleration can affect interparticle spacing. We also studied the role of rotational speed on the crystallinity of the particle configurations and showed how fine tuning of rotational speed can generate large scale monolayer crystalline formations of nanoparticles.

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Joshi, Suvid. "MIXED SURFACTANT SYSTEMS: THERMODYNAMICS AND APPLICATIONS IN METAL OXIDE IMPRINTING." UKnowledge, 2014. http://uknowledge.uky.edu/cme_etds/29.

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In this work we study mixtures of cationic surfactant (CTAB) and sugar based surfactant(s) (octyl beta-D-glucopyranoside (C8G1), dodecyl maltoside (C12G2) and octyl beta-D-xylopyranoside (C8X1)) to understand the non-ideal thermodynamic behavior of the mixtures of cationic and non-ionic surfactants in water and synthesis of imprinted materials. The thermodynamics of micellization, mixing and dilution of these systems are studied using Isothermal Titration Calorimetry (ITC) and the experimental data obtained are modeled with a pseudo-phase separation model with non-ideal mixing described by regular solution theory. It is shown that a model accounting for enthalpy of demicellization and enthalpy of dilution based on McMillan-Mayer model is able to fit ITC data set for CTAB-C8G1 system with varying mole fractions. In addition to measuring non-ideal mixing behavior, mixtures of cationic and saccharide-based surfactants are of interest for the molecular imprinting of oxide materials. Mixtures of CTAB and either C8G1 or C8X1 are utilized to prepare nonporous adsorbent materials which act as selective adsorbents towards the headgroup of the saccharide surfactant. The approach is based on the Stöber silica particle synthesis process in which surfactants are added to soft particles present at the onset of turbidity to imprint their surface. This approach is shown to yield particles displaying selective adsorption for sugars with different number of carbons, but also provide enantioselective adsorption of targeted saccharides. Enantioselectivity of D-glucose, D-xylose and D-maltose is demonstrated by imprinting with C8G1, C8X1 and C12G2, respectively. The imprinting technique provides the first example of selective adsorption based on non-covalent imprinting of silica for sugars. The mixed surfactant are also used to synthesize templated porous materials incorporating titanium which are used for epoxidation catalysis. The porous materials obtained have high surface area, uniform pore sizes in the mesopore range, and provided high selectivity and activity towards epoxidation of styrene. Titanosilicate thin films are also synthesized using cationic and saccharide surfactant mixtures to understand the incorporation of the titanium into the porous material. It is demonstrated that large amounts of isolated, tetracoordinated titanium sites can be incorporated into mesoporous silica-based materials via the complexation of the titanium precursor with a saccharide-based surfactant.

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Kätzel, Uwe. "Dynamic Light Scattering for the Characterization of Polydisperse Fractal Systems by the Example of Pyrogenic Silica." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2007. http://nbn-resolving.de/urn:nbn:de:swb:14-1197634640783-66357.

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Dynamic light scattering (DLS) is a method to size submicron particles by measuring their thermal motion (diffusion) in suspensions and emulsions. However, the validity of the Stokes-Einstein equation that relates the diffusion coefficient and the particle size is limited to spherical particles and very low concentrations. Within this thesis, DLS is used for the characterization of suspensions of pyrogenic silica which consists of fractal-like aggregates composed of sintered spherical primary particles. These structural features clearly complicate the understanding of DLS experiments and have been a severe obstacle to employing DLS as routine standard tool for the characterization of pyrogenic silica. The main objective of this thesis is therefore to evaluate the application of DLS in product development and quality assurance of pyrogenic silica industry, what essentially means to identify those structural properties of fractal aggregates which are measurable with DLS and to quantify the method’s sensitivity to changes in these properties. The investigations presented here are split up into four parts, simulations that establish a relation between structural and hydrodynamic properties, experiments validating the simulation results, the characterization of concentrated suspensions and the application-oriented analysis of DLS data for specific industrially relevant measurement tasks
Die Dynamische Lichtstreuung (DLS) ist eine Messmethode zur Größenbestimmung submikroner Partikel. Dabei wird primär die stochastische Bewegung der Teilchen (Diffusion) in Suspensionen und Emulsionen bewertet. Die Stokes-Einstein Gleichung, die das Verhältnis zwischen gemessenem Diffusionskoeffizienten und Partikelgröße wiedergibt, ist jedoch nur für kugelförmige Teilchen, die in sehr niedriger Konzentration vorliegen, gültig. In der vorliegenden Arbeit wird die dynamische Lichtstreuung zur Charakterisierung von Suspensionen pyrogener Kieselsäure eingesetzt. Diese besteht aus fraktalen Aggregaten, die wiederum aus versinterten aber meist kugelförmigen Primärpartikeln zusammengesetzt sind. Diese strukturellen Eigenschaften erschweren die Anwendbarkeit der DLS bzw. die Interpretation der Messergebnisse und verhinderten bisher den Einsatz der DLS als Routinemethode zur Charakterisierung pyrogener Kieselsäuren. Das Hauptziel dieser Arbeit ist daher eine Bewertung der Möglichkeiten der DLS für die Produktentwicklung und Qualitätssicherung in der Herstellung pyrogener Kieselsäuren. Das bedeutet im Besonderen, dass sowohl die messbaren granulometrischen Eigenschaften als auch die Sensitivität der Methode bei Eigenschaftsänderungen ermittelt werden müssen. Die hier durchgeführten Arbeiten sind in vier Teile gegliedert: Simulationen, die eine Beziehung zwischen strukturellen und hydrodynamischen Eigenschaften herstellen, Experimente zur Validierung der Simulationsergebnisse, die Charakterisierung konzentrierter Suspensionen und die anwendungsorientierte Auswertung von DLS-Daten für spezifische industrierelevante Messaufgaben

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Kätzel, Uwe. "Dynamic Light Scattering for the Characterization of Polydisperse Fractal Systems by the Example of Pyrogenic Silica." [S.l. : s.n.], 2007. http://nbn-resolving.de/urn:nbn:de:swb:14-1197634640783-66357.

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Kailasam, Varadharajan. "The removal and recovery of oxo-anions from aqueous systems using nano-porous silica polyamine composites." Diss., [Missoula, Mont.] : The University of Montana, 2009. http://etd.lib.umt.edu/theses/available/etd-08312009-114629.

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Deyhim, Sina. "Deriving Gas Transport Properties of Microporous Silica Membranes from First Principles and Simulating Separation of Multi-Component Systems in Different Flow Configurations." Thesis, Université d'Ottawa / University of Ottawa, 2014. http://hdl.handle.net/10393/31340.

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Amorphous silica membranes have molecular sieving properties for the separation of hydrogen from gas mixtures at high temperature. Consequently, they are considered to be applied in separation of a shifted syngas coming out of a water-gas-shift-reactor into the syngas and hydrogen. This separation is a key to an Integrated Gasification Combined Cycle (IGCC) plant, which would allow reducing the carbon footprint in power generation industry. The main objective of this thesis was to carry out a preliminary assessment of suitability of currently available amorphous silica membranes for this separation. However, the separation properties of amorphous silica membranes reported in the open literature vary by orders of magnitude. Therefore, in the first part of this thesis the separation properties of hypothetical silica membrane with different pore size distributions were predicted from first principles. Considering different possible gas transport mechanisms, it was concluded that gas transport in amorphous silica membranes is dominated by the activated and non-activated Knudsen diffusion. The activation energy for transport of different species was predicted using the concept of suction energy. Then, with arbitrary pore size distributions gas permeance of hypothetical silica membrane was predicted for different gas species. Since the pore size distribution of amorphous silica membrane cannot be known a priori, the developed model was used to determine the pore size distribution based on experimentally measured single gas permeances of three different species (kindly provided by Natural Resources Canada, CANMET Energy Technology Center (CETC) laboratory in Ottawa) by minimizing the error of the calculated permeance ratios with respect to the experimental values. The results indicate that, depending on how the objective function is defined, more than one pore size distribution can be found to satisfy the experimental permeance ratios. It is speculated that by increasing the number of experimentally determined permeances, a more unique pore size distribution for the tested silica membrane can be obtained. However, even at this early stage, the developed model provides a rational explanation for the effect of membrane densification on the properties of silica membranes. More specifically, a simultaneous decrease in membrane permeance and selectivity due to membrane densification, reported in the literature, is explained by shrinking the size of pores beyond a certain critical value, which depends on the kinetic diameter of gas molecules that are being separated. Comparing theoretically determined permeances, which match experimentally observed permeance ratios, revealed that the experimental permeances are considerably smaller than the theoretical values. The ratio of the two provided the basis for a scaling factor, a new concept that was introduced in this thesis. To simulate membrane module performance, a novel approach was introduced. More specifically, co- and counter-current flow configurations as well as cross-flow configuration were modeled by assuming no change in feed composition over an infinitesimally small element of membrane area. This led to a system of linear, rather than differential equations, which was readily solved numerically.

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Davis, Christina Clarkson. "Aqueous Silica in the Environment: Effects on Iron Hydroxide Surface Chemistry and Implications for Natural and Engineered Systems." Thesis, Virginia Tech, 2000. http://hdl.handle.net/10919/33948.

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Aqueous silica is present in all natural waters and exhibits a high affinity for the surfaces of iron oxides. Therefore, it is expected to play an important role in environmental systems. Experiments were conducted to investigate the fundamentals of silica sorption onto pre-formed ferric hydroxide at pH 5.0-9.5 and silica concentrations of 0-200 mg/L as SiO₂. Over the entire pH range studied, sorption densities exceeding monolayer sorption were observed at silica levels typical of natural waters. Under some circumstances, sorption exceeded a monolayer while the particle zeta potential remained positive, a phenomenon which is inconsistent with available models. To address this deficiency, an extended surface complexation model was formulated in which soluble dimeric silica sorbs directly to iron surface sites. This model fits sorption density data up to 0.40 mol SiO₂/mol Fe, and it accurately predicts trends in zeta potential and the observed H⁺ release during silica sorption to ferric hydroxide at pH 5.0 and 6.0.

A second phase of research was aimed at identifying the practical implications of silica sorption to iron hydroxide in natural and engineered systems. Two types of surfaces were prepared by exposing pre-formed Fe(OH)₃ to aqueous silica (0-200 mg/L as SiO₂) for periods of 1.5 hours or 50 days. The concentration of pre-formed iron passing through a 0.45 micron pore size filter at pH 6.0-9.5 increased as the solids aged in the presence of silica. Consistent with formation of small, stable colloids, "soluble" iron concentrations exceeded 0.2 mg/L only at zeta potentials < -15 mV. When arsenate was added to iron hydroxide particles equilibrated with silica for 1.5 hours, percentage arsenate removals were high. In contrast, arsenate removals decreased markedly as pH and silica concentrations increased if silica was pre-equilibrated with the iron for 50 days. Trends in percentage removal of humic substances were similar. Competition for sorption sites was the main cause of hindered anionic contaminant removal. However, interference with hydrolysis and precipitation are expected to be important under some circumstances, particularly during water treatment.
Master of Science

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Gutierrez, Cuevas Karla Guadalupe Gutierrez. "LIQUID CRYSTALLINE NANOCOMPOSITES: FROM ACHIRAL TO CHIRAL SYSTEMS." Kent State University / OhioLINK, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=kent1500998489695319.

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SA, LUCAS TORRES MIRANDA. "SYNTHESIS, CHARACTERIZATION AND EVALUATION OF DRUG DELIVERY SYSTEMS BASED ON MESOPOROUS SILICA FOR IMAGE IN NUCLEAR MEDICINE." PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO, 2012. http://www.maxwell.vrac.puc-rio.br/Busca_etds.php?strSecao=resultado&nrSeq=20339@1.

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PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO
CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO
O câncer é a segunda maior causa de morte no mundo inteiro e estima-se que até 2030, serão 27 milhões de novos casos e 17 milhões de mortes. Devido a esse fato, o desenvolvimento de novos sistemas de liberação (Drug delivery systems - DDS) que permitam a distribuição de um agente bioativo no seu sítio terapêutico na dose certa, numa taxa específica, acarretando menor toxicidade, e que possa ser utilizado tanto para o tratamento como para o diagnóstico de enfermidades. Atualmente, as sílicas mesoporosa surgem como potenciais DDS ou carreadores em radiofármacos, devido a sua estrutura organizada, alta área superficial e tamanhos e volumes de poros ajustáveis. Nesse trabalho foram sintetizados três potencias sistemas de liberação ou carreadores para radiofármacos para exames de imagem em medicina nuclear. A SBA-15 e sua associação com a hidroxiapatita (HAP) por dois métodos diferentes: adição dos precursores durante formação da mesofase (SBA-15/HAP_1) e o segundo por impregnação na estrutura da SBA-15 já sintetizada e calcinada (SBA-15/HAP_2). Os materiais foram marcados com o radioisótopo 99mTc e tiveram suas marcações e biodistribuições avaliadas. A SBA-15 também foi conjugada com o aptâmero anti-MUC1 para realização de direcionamento ativo para células tumorais. Os materiais foram caracterizados por: espectroscopia de emissão ótica por plasma acoplado indutivamente (ICP-OES); análise termogravimétrica (ATG); fisissorção de nitrogênio; difração de raios-X (DRX); infravermelho (IV); microscopia eletrônica de transmissão e varredura (MET e MEV); e difração a laser. As avaliações da marcação e da biodistribuição foram realizadas por contador de raios gama e gama-câmara respectivamente. A SBA-15 apresentou uma estrutura mesoporosa altamente ordenada, com alta área superficial. Os materiais impregnados com hidroxiapatita apresentaram diferenças estruturais: Na SBA-15/HAP_1 houve bloqueio quase total dos mesoporos com nanopartículas de hidroxiapatita, enquanto na SBA-15/HAP_2, houve um bloqueio parcial dos mesoporos, apresentando também agregados de hidroxiapatita. A metodologia de marcação com o 99mTc apresentou estabilidade de 8 horas. A conjugação da SBA-15 com o aptâmero anti-MUC1 apresentou maior reconhecimento das partículas de SBA-15 por células tumorais.
Cancer is the second major leading cause of death worldwide and is estimated till 2030, 27 million new cases and 17 million of deaths. So, the development of new drug delivery systems (DDS) that allows a bioactive agent distribution in its therapeutic site in the right dose, in a specific rate, leading lower toxicity, and that can be used for treatment and diagnosis of several diseases. Recently, mesoporous silicas arise as promising DDS or carriers for radiopharmaceuticals, because of its highly organized structure, high superficial area and tunable pore size and volumes. In this work, were synthesized three potential DDS or carriers for radiopharmaceuticals for imaging in nuclear medicine. SBA-15 and its association with hydroxyapatite (HAP) by two distinct methodologies: precursors addition during mesophase formation (SBA-15/HAP_1); and precursors impregnation in SBA-15 previously synthesized and calcined (SBA-15/HAP_2). The materials were labelled with tecnecium-99m radioisotope and its labeling methodology and biodistribution were evaluated. SBA-15 was also conjugated with the aptamer Anti-MUC1 for active delivery to tumoral cells. The materials were characterized by: inductively coupled plasma optical emission spectroscopy (ICP-OES); thermogravimetric analysis (TGA); nitrogen physisorption; x-ray diffraction (DRX); infrared (IR), transmission and scanning electronic microscopy (TEM and SEM); and laser diffraction. The labeling and biodistribution evaluation were performed by gamma-ray counter and gamma-camera respectively. The materials were synthesized and have shown peculiar characteristics. SBA-15 has highly ordered mesoporous structure with high superficial area. The materials impregnated with hydroxyapatite showed structural differences: In SBA-15/HAP_1, hydroxyapatite nanocrystals almost blocked the entire mesopores, while in SBA-15/HAP_2, there were a partially blocking of the mesopores and also presented hydroxyapatite nanocrystals aggregates. The tecnecium-99m labeling methodology of the materials showed an 8 hours stability. SBA-15 conjugation with Anti-MUC1 for active delivery has shown a better recognition by tumor cells.

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Cole, Robert Paul. "Ballistic Penetration of a Sandbagged Redoubt Using Silica Sand and Pulverized Rubber of Various Grain Sizes." Scholar Commons, 2010. http://scholarcommons.usf.edu/etd/3565.

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The basis of this work is to find how varying the grain size of materials contained in sandbags (sand and crumb rubber) effects the ballistic penetration of the projectiles from both the 7.62x39mm (308-short), and 9mm Luger cartridges. The sandbags were stacked in a pyramidal stacking configuration according to military specifications in order to simulate a section of a sandbag barrier or redoubt as would be seen on the battlefield. The projectiles were fired at the targets, and the velocity and penetration data was recorded. The results concern both military and civilian applications alike. The 7.62x39 round was found to experience more fragmentation as grain size increased, and was also found to have, on average, the least amount of penetration into the largest grains. The 9mm round was found to suffer negligible deformation in all of the various sizes of materials, and when fired at the two types of materials, showed a steady trend of decreasing penetration depth with increasing grain size. The sand had a wearing effect on the projectiles leaving them scared or fragmented and deformed while the rubber kept the rounds in pristine condition.

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Ribes, Llop Susana. "Study of different antifungal systems to preserve strawberry jams against fungi spoilage." Doctoral thesis, Universitat Politècnica de València, 2017. http://hdl.handle.net/10251/82306.

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New tendencies in the development of innovative food packages could affect product microbial stability during storage. In this sense, antifungal systems such as emulsions, nanoemulsions and mesoporous silica supports, may be promising alternatives to preserve the product quality without having to apply further thermal treatments. The formulation of stable antifungal systems and the optimisation of the methodology to be employed to prepare these systems play an important role in: i) their antifungal effectiveness; ii) bioactive compounds losses during their preparation; and iii) their impact on the food product's sensory profile. Nanoemulsions prepared with essential oils generally presented higher antifungal effect than free essential oils applied at the same concentrations. Furthermore, the emulsifier played a key role in the resulting antifungal activity. Whey protein isolated-based nanoemulsions were more effective in inhibiting mycelial mould growth and spore germination than Tween 80-based ones. The great in vitro effectiveness of nanoemulsions to control mould development allowed to check their application to food products, and strawberry jam was selected as the food matrix. To this end, clove and cinnamon leaf emulsions were incorporated into strawberry jams to control fungal decay. Although these emulsions were able to reduce jam spoilage, their incorporation negatively affected the aroma, taste and the overall acceptance of the jam. Regarding the methodology employed to prepare oil-in-water emulsions, the magnetic stirring and high pressure homogenisation combination was the most effective to reduce essential oil losses. Moreover, stable cinnamon bark-xanthan gum emulsions with good in vitro antifungal properties against the target fungi were obtained. Despite the promising use of cinnamon bark emulsions to control fungi decay in strawberry jam, their incorporation negatively affected the product's aroma, taste and overall acceptance. Given the strong impact of essential oils on the food product's sensory profile, two new approaches were investigated: i) combinations of different antifungal compounds in emulsions; and ii) immobilisation of bioactive compounds on mesoporous silica surfaces. The cinnamon bark essential oil, zinc gluconate and trans-ferulic acid combination allowed the obtention of a product considered microbiologically acceptable and with good organoleptic characteristics. However, total mould inhibition was not achieved. Consequently, the antifungal and sensory properties of the bioactive agents (eugenol and thymol) immobilised on mesoporous silica surfaces were studied. The preparation of jams with eugenol immobilised on MCM-41 microparticles induced better control of the fungal inhibition compared with the samples functionalised with thymol. The sensory analysis of the jams after incorporating the solids revealed that eugenol and thymol immobilisation cushioned the impact of these compounds on the jam flavour profile.
Las nuevas tendencias en el desarrollo de envases alimentarios innovadores podrían afectar a la estabilidad microbiana del producto durante el almacenamiento. En este sentido, sistemas antifúngicos tales como emulsiones, nanoemulsiones y soportes mesoporosos de sílice pueden ser alternativas prometedoras para preservar la calidad del producto sin tener que aplicar otros tratamientos térmicos. La formulación de sistemas antifúngicos estables y la optimización de la metodología a emplear para preparar estos sistemas, tienen un papel importante en: i) su eficacia antifúngica; ii) pérdidas de los compuestos bioactivos producidas durante su preparación; y iii) su impacto en el perfil sensorial del producto alimenticio. Las nanoemulsiones preparadas con aceites esenciales presentaron por norma general un mayor efecto antifúngico que los aceites libres aplicados a las mismas concentraciones. Asimismo, el tipo de emulsionante utilizado desempeñó un papel clave en la actividad antifúngica de las nanoemulsiones. Las nanoemulsiones preparadas con proteína de suero de leche fueron más eficaces en la inhibición del crecimiento micelial y en la germinación de las esporas que las formuladas con Tween 80. La gran eficacia in vitro de las nanoemulsiones en el control del desarrollo de moho permitió evaluar su aplicación en productos alimenticios, siendo seleccionada la confitura de fresa como matriz alimenticia. Con este fin, las emulsiones de los aceites esenciales de clavo y de hoja de canela fueron incorporadas a las confituras de fresa con el fin de controlar el deterioro fúngico. A pesar de que estas emulsiones fueron capaces de reducir el deterioro fúngico de las confituras de fresa, su incorporación afectó negativamente al aroma, el sabor y la aceptación global de la confitura. En cuanto a la metodología empleada para preparar emulsiones aceite-agua, la combinación de agitación magnética y homogeneización por altas presiones fue la más eficaz para reducir las pérdidas de aceite esencial. Asimismo, se obtuvieron emulsiones estables con una alta capacidad antifúngica, determinada in vitro, frente a los hongos objeto de estudio. A pesar del prometedor uso de las emulsiones de aceite esencial de la corteza de canela en el control del deterioro fúngico de las confituras de fresa, su incorporación al alimento afectó negativamente al aroma, sabor y aceptación global del producto. Debido al gran impacto de los aceites esenciales en el perfil sensorial del producto alimenticio, se investigaron dos nuevos enfoques: i) combinaciones de diferentes compuestos antifúngicos en emulsiones; y ii) inmovilización de compuestos bioactivos sobre superficies de sílice mesoporosas. La combinación de aceite esencial de corteza de canela, el gluconato de zinc y el ácido trans-ferúlico permitió la obtención de un producto considerado microbiológicamente aceptable con buenas características organolépticas pero no se consiguió la inhibición total del crecimiento de moho. Por ello, se estudiaron las propiedades antifúngicas y sensoriales de agentes bioactivos (eugenol y timol) inmovilizados sobre superficies de sílice mesoporosas. La preparación de las confituras con eugenol inmovilizado en las micropartículas de MCM-41, mostró un mejor control de la inhibición fúngica en comparación con las muestras preparadas con timol funcionalizado. El análisis sensorial de las muestras tras la incorporación de los sólidos a la confitura de fresa, reveló que la inmovilización de eugenol y timol reduce el impacto sensorial de estos compuestos en confituras de fresa.
Les noves tendències en el desenvolupament d'envasos alimentaris innovadors podrien afectar l'estabilitat microbiana del producte durant l'emmagatzematge. En aquest sentit, sistemes antifúngics com les emulsions, nanoemulsions i suports mesoporosos de sílice poden ser alternatives prometedores per preservar la qualitat del producte sense haver d'aplicar altres tractaments tèrmics. La formulació de sistemes antifúngics estables, així com l'optimització de la metodologia a emprar per preparar aquests sistemes, tenen un paper important en: i) la seva eficàcia antifúngica; ii) pèrdues dels compostos bioactius produïdes durant la seva preparació; i iii) el seu impacte en el perfil sensorial del producte alimentari. Les nanoemulsions preparades amb olis essencials van presentar per norma general, un major efecte antifúngic que els olis lliures aplicats a les mateixes concentracions. Així mateix, el tipus d'emulsionant utilitzat va tenir un paper clau en l'activitat antifúngica de les nanoemulsions. Les nanoemulsions preparades amb proteïna de sèrum de llet van ser més efectives en la inhibició del creixement micelial i en la germinació de les espores que les formulades amb Tween 80. La gran eficàcia in vitro de les nanoemulsions en el control del desenvolupament de fongs va permetre avaluar la seva aplicació a productes alimentaris, sent seleccionada la confitura de maduixa com a matriu alimentària. Amb aquesta finalitat, les emulsions dels olis essencials de clau i de fulla de canyella van ser incorporades a les confitures de maduixa per tal de controlar el deteriorament fúngic. Tot i que aquestes emulsions reduïren el deteriorament fungic de les confitures de maduixa, la seva incorporació va afectar negativament a l'aroma, el sabor i l'acceptació global de la confitura. Pel que fa a la metodologia emprada per preparar emulsions oli-aigua, la combinació d'agitació magnètica i homogeneïtzació per altes pressions va ser la més eficaç per reduir les pèrdues d'oli essencial. A més, es van obtenir emulsions estables amb una alta capacitat antifúngica, determinada in vitro, davant dels fongs objecte d'estudi. Malgrat el prometedor ús de les emulsions d'oli essencial de l'escorça de canyella en el control del deteriori fúngic de les confitures de maduixa, la seva incorporació a l'aliment va afectar negativament a l'aroma, sabor i acceptació global del producte. A causa del gran impacte dels olis essencials en el perfil sensorial del producte alimentari, es van investigar dos nous enfocaments: i) combinacions de diferents compostos antifúngics en les emulsions; i ii) immobilització de compostos bioactius sobre superfícies de sílice mesoporoses. La combinació d'oli essencial d'escorça de canyella, el gluconat de zinc i l'àcid trans-ferúlic va permetre l'obtenció d'un producte considerat microbiològicament acceptable amb bones característiques organolèptiques però no es va aconseguir la inhibició total del creixement del fong. Per això, es van estudiar les propietats antifúngiques i sensorials d'agents bioactius (eugenol i timol) immobilitzats sobre superfícies de sílice mesoporoses. La preparació de les confitures amb eugenol immobilitzat en les micropartícules de MCM-41, va mostrar un millor control de la inhibició fúngica en comparació amb les mostres preparades amb timol funcionalitzat. L'anàlisi sensorial de les mostres després de la incorporació dels sòlids a la confitura de maduixa, va revelar que la immobilització de eugenol i timol redueix l'impacte sensorial d'aquests compostos en confitures de maduixa.
Ribes Llop, S. (2017). Study of different antifungal systems to preserve strawberry jams against fungi spoilage [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/82306
TESIS
Premiado

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31

Schmidt, Alexandra [Verfasser], and Thomas [Akademischer Betreuer] Bein. "Synthesis and functionalization of mesoporous silica materials for applications as host-guest-systems / Alexandra Schmidt. Betreuer: Thomas Bein." München : Universitätsbibliothek der Ludwig-Maximilians-Universität, 2014. http://d-nb.info/1080479228/34.

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Bouledjouidja, Abir. "Imprégnation supercritique pour l'élaboration de systèmes à libération prolongée." Thesis, Aix-Marseille, 2016. http://www.theses.fr/2016AIXM4303/document.

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Le procédé d’imprégnation en milieu supercritique est une alternative « propre » à l’imprégnation par voie liquide. Entre autres applications, les procédés d’imprégnation peuvent être utilisés pour l’élaboration de systèmes de délivrance de médicaments appliqués aux domaines pharmaceutique et médical. Cette étude porte sur l’élaboration de systèmes de délivrance de médicaments en utilisant l'imprégnation supercritique des principes actifs sur deux types de supports : des matrices polymériques (lentilles intraoculaires) et des matrices poreuses (silices mésoporeuses). Dans le premier cas, des lentilles polymériques intraoculaires (IOLs), utilisées pour la chirurgie de la cataracte, ont été imprégnées par des principes actifs : un anti-inflammatoire (Dexaméthasone 21-phosphate disodium: DXP) et un antibiotique (Ciprofloxacine: CIP). Plus particulièrement, deux types de lentilles ont été étudiés : des IOLs rigides à base de PMMA et des IOLs souples à base de P-HEMA. Les expériences d'imprégnation supercritique ont été effectuées en mode batch et les taux d'imprégnation ont été déterminés par des études de cinétique de relargage des principes actifs. L’influence des conditions opératoires sur l’efficacité de l’imprégnation a été étudiée en réalisant des expériences d’imprégnation préliminaires suivies par des plans d’expériences par la suite. Dans le second cas, une silice mésoporeuse a été utilisée comme support d’imprégnation pour un médicament faiblement hydrosoluble (Fénofibrate), afin d’augmenter sa cinétique de dissolution. L’imprégnation supercritique a été effectuée avec le CO2 pur en faisant varier la pression et le taux de dépressurisation (rapide et lent)
Supercritical impregnation is an attractive “clean” alternative to conventional impregnation processes using generally liquid organic solvents. Among other applications, the impregnation process can be used for the development of controlled drug delivery systems applied to the pharmaceutical and medical fields. This work focuses on the preparation of controlled drug delivery systems using supercritical impregnation of drugs in two kinds of impregnation supports: polymeric matrices (intraocular lenses) and porous supports (mesoporous silica). Firstly, the supercritical impregnation of polymeric intraocular lenses (IOLs), used in cataract surgery, by an anti-inflammatory drug (Dexamethasone 21-phosphate disodium: DXP) and an antibiotic (Ciprofloxacin: CIP), is studied. More particularly, two polymeric IOLs were tested: rigid intraocular lenses made from derivative of PMMA and foldable intraocular lenses made from derivative of P-HEMA. Supercritical impregnations were carried out in a batch mode and the impregnation yields were determined through drug release kinetics studies in a solution simulating the aqueous humor. The influence of operating conditions on impregnation was studied by performing preliminary impregnation experiments followed by experimental designs. The second part of this work deals with the loading of a poorly water-soluble drug (Fenofibrate) in a mesoporous silica for improving drug dissolution kinetics. Supercritical impregnations were carried out with pure CO2 at different pressures (100 to 200 bar) and depressurization rates (rapid and slow)

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Oliveira, Fernando Jose Volpi Eusebio de. "Hibridos inorganico-organicos mesoporosos nanoestruturados = aspectos estruturais e energeticos das interações cations-centros basicos na interface solido/liquido." [s.n.], 2009. http://repositorio.unicamp.br/jspui/handle/REPOSIP/250026.

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Orientador: Claudio Airoldi
Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Quimica
Made available in DSpace on 2018-08-15T02:31:23Z (GMT). No. of bitstreams: 1 Oliveira_FernandoJoseVolpiEusebiode_D.pdf: 14034511 bytes, checksum: befefa4bb08edceee361642b479a35ca (MD5) Previous issue date: 2009
Resumo: Três conjuntos de sílicas mesoporosas foram sintetizados com os agentes direcionadores dodecilamina, brometo de cetiltrimetilamônio (CTAB) e co-polímero tribloco EO20-PO70-EO20 (P123 ¿ Pluronic®). As matrizes inorgânicas foram funcionalizadas com agentes sililantes contendo de um a três átomos de nitrogênio nas cadeias. Além disso, estes silanos reagiram com o ligante tiocarbamida, em uma etapa livre de solvente, anteriormente à formação da sílica, em processo de co-condensação. A rota de síntese empregada para as amostras preparadas a partir do direcionador P123 foi a pósfuncionalização. Para as estruturas obtidas utilizando-se dodecilamina, do tipo HMS, observou-se o colapso da estrutura após a extração do direcionador, conforme mostraram os espectros de IV e os difratogramas antes e depois do processo de remoção. Contudo, as amostras apresentaram tamanho médio de poros na faixa que constituem os materiais mesoporosos, sendo então investigados no estudo da remoção de metais tóxicos. Para as amostras preparadas CTAB e P123 foram observados os sinais da reflexão típica de materiais do grupo p6mm, denominada 2D-hexagonal, cujas amostras análogas aos materiais MCM-41 e SBA-15, respectivamente. Todos os híbridos modificados com tiocarbamida foram aplicados em sorção de íons metálicos, ajustados ao modelo não linear de sorção de Langmuir. As interações na interface sólido/líquido foram determinadas por microcalorimetria. Os resultados revelaram que os materiais do tipo SBA-15 apresentam alta capacidade de remoção de Cu, Cd e Pb, devido ao procedimento de pós-funcionalização. As amostras obtidas por co-condensação, do tipo HMS e MCM-41, apresentaram capacidade máxima de sorção superior aos resultados observados na literatura para materiais análogos. Os experimentos calorimétricos mostraram que as interações entre os sólidos e os íons metálicos são exotérmicas, com exceção dos íons Pb. Outro aspecto destacado trata-se da importância do termo entrópico, que parece reger o processo na maioria dos casos, devido à liberação de moléculas de água coordenadas aos íons e às matrizes. Portanto, todos os sistemas estudados apresentaram um comportamento energeticamente favorável.
Abstract: Three set of mesoporous silicas have been synthesized through dodecylamine, cetiltrimethylamonium bromide (CTAB) and the triblock co-polymer EO20-PO70-EO20 (P123 ¿ Pluronic®) as structure directing agents (sda). The inorganic matrices have been functionalized with silylating agents presenting from one to three nitrogen atoms on their chains. In addition, these silanes reacted with thiocarbamide through a free-solvent step, before the silica formation, by co-condensation process. However the synthetic route for the samples templated by P123 was the post-grafting. For the structures obtained by using dodecylamine, HMS-like, it was observed the structure collapsed after template removal, as shown by IR spectra and XRD patterns, before and after the removal process. These samples presented pore size comprised on mesoporous range, being then investigated for toxic metal removal capacity. For the samples prepared from CTAB and P123, the typical reflections for p6mm group materials, named 2D-hexagonal, were observed, and these samples are analogous to MCM-41 and SBA-15 materials, respectively. All thiocarbamide-modified hybrids were applied to metal ions sorption, being adjusted to Langmuir non-linear fit model. The interactions at the solid/liquid interface were determined through microcalorimetry. The results reveal that the SBA-15-like materials present high removal capacity for Cu, Cd e Pb, due to the post-grafting procedure. The samples obtained through cocondensation route, HMS- and MCM-41-like, presented maximum sorption capacity higher than those results for analogous published materials. With exception of Pb, all calorimetric determinations showed that the interactions between the solids and metal ions are exothermic. Another highlighted feature is about the importance of the entropic term that seems to rule the processes for several cases, due to the ion and surface coordinated water molecules displacement. Thus, all studied systems presented an energetically favorable behavior.
Doutorado
Quimica Inorganica
Doutor em Ciências

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34

Alleman, Coleman. "Molecular Dynamics Investigations of Polystyrene-Based Binary Thin Film Systems: Interfacial Properties and Mechanical Behavior." The Ohio State University, 2011. http://rave.ohiolink.edu/etdc/view?acc_num=osu1306909005.

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35

Goursaud, Matthieu. "Contribution to the development of nano-systems for the recognition of fluoride in water." Doctoral thesis, Universite Libre de Bruxelles, 2013. http://hdl.handle.net/2013/ULB-DIPOT:oai:dipot.ulb.ac.be:2013/209378.

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The development of molecular receptors for anion recognition has become an important aspect of supramolecular chemistry. In this thesis, we focused our attention to the study of systems for fluoride recognition in water. Fluoride is indeed an anion of interest due to its implication in environmental and health related issues. Furthermore, its small size and high hydration energy make its recognition in water particularly challenging.

Most of the synthetic systems reported for fluoride recognition have been extensively studied in organic solvents (DMSO, acetonitrile) using tetrabutylammonium fluoride (TBAF) as the source of fluoride. In many cases, titra- tion behaviours are observed that cannot be ascribed to a classical 1:1 binding isotherm, deprotonation problems of Brønsted-Lowry acid type of receptors aside. In the first part of our thesis we investigated, using a uranyl-salophen re- ceptor which recognizes fluoride via Lewis Acide/Base interactions, the origin of the unusual titration behaviour. Via UV/vis, 19F and 1H NMR spectroscopies, we have been able to highlight that the equilibrium between the fluoride and the corresponding bihalide ion, HF−2 ,which is inevitably generated along with the hydroxide anion in situ due to trace amounts of water, can be at the ori- gin of this singular behaviour. Our results put to light that when undertaking titrations with fluoride in DMSO, the fluoride–bihalide equilibrium can affect the data and that the latter species can even be the dominating species at low TBAF concentrations. When varying the solvent from DMSO to acetonitrile, the s-shape titration curves observed by UV/vis are no longer observed for the uranyl-salophene receptor that we studied. The fluoride-bifluoride equilibrium is still present but both of the anions generated in this process are recognised by the uranyl-salophene receptor with similar affinity constants above 10^6 M−1.

The second part of our work was devoted to finding ways to solubilize anion receptors that are efficient in organic solvents, into an aqueous environment. Two approaches were investigated: (i) grafting of the receptors onto silica nanoparticles and (ii) the micellar incorporation of the receptors. For the first strategy, we developed two silylated urea-based receptors. These receptors were first studied in organic solvents (DMSO and/or acetonitrile) where they showed selectivity, among halides, towards fluoride. Once grafted on the silica nanoparticles, due to the fact that hydroxyl groups and solvent molecules are present in the silica matrix, fluoride recognition was not possible.

We explored it with different simple H-bond based urea receptors in the second srategy. With the cationic surfactants, cetyl trimethyl ammonium chloride and bromide, the counter-ions of the micelles interfere with the fluoride recognition. With the neutral surfactant triton X-100, the incorporation of the anion receptors proved to be difficult. Moreover, the variations observed in the UV/vis spectra upon titrations were too small to be able to make any conclusions about fluoride recognition.
Doctorat en Sciences de l'ingénieur
info:eu-repo/semantics/nonPublished

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36

Hernández, Teruel Adrián. "Smart drug delivery systems designed to improve Inflammatory Bowel Disease therapy." Doctoral thesis, Universitat Politècnica de València, 2019. http://hdl.handle.net/10251/129863.

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[ES] La presente tesis doctoral titulada "Sistemas de liberacio'n controlada de fa'rmacos diseñados para mejorar el tratamiento de Enfermedad Inflamatoria Intestinal" se centra en el diseño, preparación, caracterización y evaluación in vivo de distintos sistemas de liberación controlada de fármacos en colon (CDDS, por sus siglas en inglés) utilizando como soporte micropartículas de silice mesoporosa, funcionalizadas con puertas moleculares. En conclusión, los estudios realizados demuestran que los materiales de silice mesoporosa, en combinación con puertas moleculares sensibles a estímulos específicos, tienen un gran potencial para el desarrollo de nuevos sistemas de liberación controlada de fármacos en el colon, dirigidos a mejorar el arsenal terapéutico disponible para el tratamiento de EII. La posibilidad de adaptar o personalizar la carga y las puertas moleculares hace que estos soportes de sílice mesoporosa sean una opción interesante para el desarrollo de nuevos sistemas de liberación controlada de fármacos en diferentes aplicaciones biomédicas. Finalmente, esperamos que los resultados obtenidos en esta tesis doctoral sirvan de inspiración para el desarrollo de sistemas de liberación controlada de fármacos innovadores y cada vez más inteligentes, para su aplicación tanto en medicina como en otras áreas.
[CAT] La present tesi doctoral titulada "Sistemes d'alliberament controlat de farmacs dissenyats per a millorar el tractament de Malaltia Inflamatoria Intestinal" se centra en el disseny, preparacio, caracteritzacio i avaluacio in vivo de diferents sistemes d'alliberament controlat de farmacs en colon (*CDDS, per les seues sigles en angles) utilitzant com a suport microparticules de si'lice mesoporosa, funcionalitzades amb portes moleculars. En conclusio, els estudis realitzats demostren que els materials de si'lice mesoporosa, en combinacio amb portes moleculars sensibles a estimuls especifics, tenen un gran potencial per al desenvolupament de nous sistemes d'alliberament controlat de farmacs en el colon, dirigits a millorar l'arsenal terapeutic disponible per al tractament de MII. La possibilitat d'adaptar o personalitzar la carrega i les portes moleculars, fa que aquests suports de silice mesoporosa siguen una opcio interessant per al desenvolupament de nous sistemes d'alliberacio controlada de farmacs en diferents aplicacions biomediques. Finalment, esperem que els resultats obtinguts en aquesta tesi doctoral servisquen d'inspiracio per al desenvolupament de sistemes d'alliberament controlat de farmacs innovadors i cada vegada mes intel·ligents, per a la seua aplicacio tant en medicina com en altres arees.
[EN] This PhD thesis entitled "Smart drug delivery systems designed to improve Inflammatory Bowel Disease therapy" is focused on the design, synthesis, characterization and in vivo evaluation of several Colon Drug Delivery Systems (CDDS) using hybrid mesoporous silica microparticles as scaffolds containing molecular gates. In conclusion, the studies shown in this Thesis demonstrate that mesoporous silica materials in combination with responsive molecular gates have great potential in the design and preparation of new CDDS to improve the therapeutic options available for IBD. The possibility to adapt the cargo and the molecular gate makes mesoporous silica support especially appealing for similar controlled drug delivery applications in the biomedical field. We hope that the obtained results could inspire the development of new innovative smart drug delivery systems in this or other fields.
We thank the Spanish Government (projects MAT2015-64139-C4-1-R and AGL2015-70235-C2-2-R (MINECO/FEDER)) and the Generalitat Valenciana (project PROMETEOII/2014/047) for support. AHT thanks to the Spanish MEC for his FPU grant. We thank the Generalitat Valenciana (Project PROMETEO2018/024)
Hernández Teruel, A. (2019). Smart drug delivery systems designed to improve Inflammatory Bowel Disease therapy [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/129863
TESIS

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Hecht, Mandy. "Particulate systems and thin-film based platforms." Doctoral thesis, Humboldt-Universität zu Berlin, Mathematisch-Naturwissenschaftliche Fakultät, 2015. http://dx.doi.org/10.18452/17329.

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Die Verbindung von hoch entwickelten Nanomaterialien mit fluoreszenzbasierten Technologien hat sich zu einem aufstrebenden Forschungsbereich entwickelt. Nichtsdestotrotz ist bis heute der Schritt von einem organischen Indikatormolekül zum anwendbaren Sensorsystem ein komplexer Prozess. Diese Arbeit zielte darauf ab, sensorische Materialien verschiedener chemischer Natur für diverse Analyten zu entwickeln, zu charakterisieren und zu etablieren. Hierbei wurden zunächst pH sensitive Fluoreszenzfarbstoffe entwickelt und in dünnen Membranen immobilisiert. Der Teststreifen ermöglicht die Beurteilung von pH-Änderungen mit dem Auge. Darüber hinaus wurde gezeigt, wie diese Farbstoffe auch in eine wasserlösliche Form überführt werden können. Damit konnten lokale pH-Änderungen an der Wachstumsfront von Silikat-Biomorphs detektiert werden. Auch partikuläre Systeme stellten sich als geeignete Materialien heraus. Es konnte gezeigt werden, wie die Silikat-Matrix von Partikeln zu verbesserten Eigenschaften für Farbstoffe führt. Mittels farbstoffbeladener Partikel konnte in einem Lateral-Flow-Assay ein schneller Nachweis von TATP etabliert werden. Ein anderer Ansatz verfolgte das Ziel des sensitiven Nachweises von Quecksilberionen in Wasser. In einem anderen System konnten Silikat-Nanopartikeln so funktionalisiert werden, dass ein sensitiver und selektiver Nachweis von Schwermetallionen und Anionen über ein Quencher-Displacement-Assay gelang. Zusätzlich wurde die einzigartige Oberfläche von Zellulosepartikeln mithilfe eines neu entwickelten Fluoreszenzfarbstoffs untersucht. Die untersuchten Materialien und Strategien zeigen, wie leicht innovative Moleküle für potentielle sensorische Systeme im wässrigen Medium auf Basis von fluoreszierenden Partikeln und dünnen Schichten geschaffen werden können. Das Verhalten der hergestellten Materialien wurde über spektroskopische Methoden evaluiert und dabei, wenn möglich, die Parameter Sensitivität, Selektivität und Ansprechzeit beurteilt.
The combination of fluorescence and nanomaterials has developed into an emerging research area. Nonetheless until now the step from an organic sensory molecule to a final sensor format is a complex endeavor. This thesis aimed at the preparation of particulate and thin-film based platforms for various analytes through combining the features of an appropriate host material with outstanding properties of dyes concomitant with sensitive fluorescence detection techniques. In particular, pH sensitive fluorescent probes were sterically immobilized into a thin membrane. The dip-stick allows the assessment upon change in pH with the eye. Especially a probe working at high basic pH range was converted into a water-soluble analogue and was directly applied at the growth front of silica biomorphs to detect local pH changes. But also particulate structures are suitable host materials. It is shown how the silica matrix of nanoparticles lead to improved optical properties for embedded dyes. The interactions of silica and fluorescent dyes within the pores of mesoporous particles were exploited to develop an actual sensor format based detection of TATP. In another approach it was possible to detect mercury ions in water. Heavy metal ions were also successfully detected in a quencher displacement assay involving receptor-dye functionalized silica nanoparticles. The impact of the unique surface properties of cellulose microparticles was shown by a fluorescent dye which allows an assessment of the surface functional groups and microenvironment through the reactivity and its changes in the optical properties. The performance of the prepared materials were evaluated mostly by spectroscopic methods and if possible assessed in terms of sensitivity, selectivity and response time. The newly developed and investigated materials based on fluorescent particulate and thin-films show the facile application of innovative sensor probes for potentially sensing devices.

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38

Junges, Fernando. "Novel catalyst systems based on Ni(II), Ti(IV), and Cr(III) complexes for oligo-and polymerization of ethylene." reponame:Biblioteca Digital de Teses e Dissertações da UFRGS, 2005. http://hdl.handle.net/10183/6358.

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Le complexe de Brookhart Ni(α-diimine)Cl2 (1) (α-diimine = 1,4-bis(2,6- diisopropylphenyl)-acenaphthenediimine) a été caractérisé après impregnation sur silice (S1) et a silices modifié avec MAO (4,0, 8,0 et 23,0 wt.% Al/SiO2 appelé S2, S3 et S4, respectivement). Le traitement de ces composés greffé avec MAO produit des catalyseurs actifs pour la polymérisation de l'éthylène. Un haute activité catalytique a été obtenue en utilisant le système supporté 1/S3 (196 kg de PE/mol[Ni].h.atm; toluene, Al/Ni = 1000, 30ºC, 60 min et pression atmosphérique d'éthylène). Les effets des conditions de la polymérisation ont été testés avec le catalyseur greffé S2 et la meilleure activité catalytique a été obtenue avec le solvant hexane, MAO comme cocatalyseur, la proportion molaire Al/Ni de 1000 et à la température de 30°C (285 kg de PE/mol[Ni].h.atm). Quand la réaction a été conduite selon la méthodologie in situ, l'activité a pratiquement doublé et les polymères ont montré des propriétés semblables. Les polymères produits par les catalyseurs supportés ont montré l'absence de température de fusion, resultats senblables à seux obtenus avec les systèms homogène par analyse DSC. En revanche, le polymères obtenus avec les système greffé presentent selon les courbes GPC une (MwD) polydispersité qui varie de 1,7 à 7,0. Un mélange de polyéthylène lineaire et ramifié (BPE/LPE) préparé utilisant les complexes Ni(α-diimine)Cl2 (1) (α-diimine = 1,4-bis(2,6-diisopropylphenyl)- acenaphthenediimine) et {TpMs*}TiCl3 (2) (TpMs* = hydridobis(3-mesitylpyrazol-1-yl)(5- mesitylpyrazol-1-yl)) greffés in situ sur silice modifiée avec MAO (4,0 wt. -% Al/SiO2, S2). Les réactions de polymérisation ont été exécutées dans le toluène à deux températures différentes (0 et 30°C), variant la fraction molaires du nickel (xNi), et utilisan MAO comme cocatalyseur externe. A toutes les températures, les activités montrent une tendence de variation linéaire avec xNi et indiquent l´absence d´effet synerque entre les espéces de nickel et du titane. Des activités les plus elèvees ont été trouvées à 0°C. Les températures de fusion pour les mélanges de polyéthylène produits à 0 °C diminuent alors que xNi augmente l'indiquant une bonne compatibilité entre les phases du polyéthylène obtenues avec les deux catalyseurs. La température de fusion des mélanges de polyéthylène dépendre de l'ordre selon lequel les catalyseurs ont été greffés sur la silice modifiée avec MAO. L'immobilisation initiale de 1 sur le support (2/1/S2) produit des polymères avec une temperature de fusion (Tm) inférieure à celle des polymère obtenus lorsque le titane a etè greffé inicialment 1/2/S2. L´observation des polyèthylènes obtenus avec les deux systèms (2/1/S2 et 1/2/S2) par microscopie electronique à balayage (SEM) a montré la formation de polymére sphérique montrant que la morphologie sphérique du support à été reproduite. Sont décrits la synthèse, la caractérisation et les propriètès catalytique pour l'oligomerization de l'éthylène de quatre composés organometalliques du CrIII possèdante les ligands (([bis[2-(3,5-dimethyl-1-pyrazolyl)ethyl]amine]chromiun(III)chloride (3a), [bis[2- (3,5-dimethyl-l-pyrazolyl)ethyl] benzylamine]chromiun(III)chloride (3b), [bis[2-(3,5- dimethyl-l-pyrazolyl)ethyl]ether] chromiun(III)chloride (3c), [bis[2-(3-phenyl-lpyrazolyl) ethyl]ether]chromiun(III)chloride (3d)). Concernent l'oligomerization, exception faite du composè 3a, tous les complexe du chrome se sont montré actif après activation avec MAO et les FR obtenues ont une effet differencie à celles atteintes avec CrCl3(thf)3. La coordination d´un ligand tridentatè sur le centre metallique ne provoque pas de changements considérables sur la formation des C4 et C6, mais la montantè de C8 est diminuèe et celles des C10 et +C12 ont ètè augmentèes. Les polymères produits par le catalyseur 3a à 3 et 20 atm d'éthylène possèdent, selon les analyses par DSC la températures de fusion de 133,8 et 136ºC respectivement. Ceci indique que dans les deux cas la production de polyèthylène de haut densité. Effectivement le masse molar moyenne, obtenus par GPC, est de 46647 g/mol avec Mw/Mn = 2,4 (3 atm). Le système 3c/MAO a montré des valeurs de FR, activité et sélectivité à α-olefins differents selon la pression d´éthylène utilisèe. Se qui montré une grand sensibilitè à la concentration d´éthylène solubilisè.
The complex of Brookhart Ni(α-diimine)Cl2 (1) (α-diimine = 1,4-bis(2,6- diisopropylphenyl)-acenaphthenediimine) has been characterized after impregnation on silica (S1) and MAO-modified silicas (4.0, 8.0 and 23.0 wts.% Al/SiO2 called S2, S3 and S4, respectively). The treatment of these heterogeneous systems with MAO produces some active catalysts for the polymerization of the ethylene. A high catalytic activity has been gotten while using the system supported 1/S3 (196 kg of PE/mol[Ni].h.atm; toluene, Al/Ni = 1000, 30ºC, 60 min and atmospheric pressure of ethylene). The effects of polymerization conditions have been tested with the catalyst supported in S2 and the best catalytic activity has been gotten with solvent hexane, MAO as cocatalyst, molar ratio Al/Ni of 1000 and to the temperature of 30°C (285 kg of PE/mol[Ni].h.atm). When the reaction has been driven according to the in situ methodology, the activity practically doubled and polymers showed some similar properties. Polymers products by the supported catalysts showed the absence of melting fusion, results similar to those gotten with the homogeneous systems by DSC analysis. But then, polymers gotten with the transplanted system present according to the GPC’s curves the polydispersity (MwD) varies between 1.7 and 7.0. A polyethylene blend (BPE/LPE) was prepared using the complex Ni(α-diimine)Cl2 (1) (α-diimine = 1,4-bis(2,6-diisopropylphenyl)-acenaphthenediimine) and {TpMs*}TiCl3 (2) (TpMs* = hydridobis(3-mesitylpyrazol-1-yl)(5-mesitylpyrazol-1-yl)) supported in situ on MAO-modified silica (4.0 wts. -% Al/SiO2, S2). Reactions of polymerization of ethylene have been executed in the toluene in two different temperatures (0 and 30°C), varying the molars fraction of nickel (xNi), and using MAO as external cocatalyst. To all temperatures, the activities show a linear variation tendency with xNi and indicate the absence of the effect synergic between the species of nickel and the titanium. The maximum of activity have been found at 0°C. The melting temperature for the blends of polyethylene produced at 0 °C decrease whereas xNi increases indicating a good compatibility between phases of the polyethylene gotten with the two catalysts. The melting temperature for the blends of polyethylene showed be depend on the order according to which catalysts have been supported on the MAO-modified silica. The initial immobilization of 1 on the support (2/1/S2) product of polymers with a melting temperature (Tm) lower to the one of the polymer gotten when the titanium has been supported inicially (1/2/S2). The observation of polyethylenes gotten with the two systems (2/1/S2 and 1/2/S2) by scanning electron microscopy (SEM) showed the spherical polymer formation showing that the spherical morphology of the support to been reproduced. Are described the synthesis, the characterization and the catalytic properties for the oligomerization of the ethylene of four organometallics compounds of CrIII with ligands ([bis[2-(3,5-dimethyl-1-pyrazolyl)ethyl]amine] chromium (III) chloride (3a), [bis[2-(3,5- dimethyl-l-pyrazolyl)ethyl]benzylamine] chromium (III) chloride (3b), [bis[2-(3,5-dimethyl-lpyrazolyl) ethyl]ether] chromiun(III)chloride (3c), [bis[2-(3-phenyl-lpyrazolyl) ethyl]ether]chromiun(III)chloride (3d)). In relation of the oligomerization, at exception made of the compounds 3a, all complex of the chromium showed be active after activation with MAO and the TOF gotten have one effect differentiated to those formed with CrCl3(thf)3. The coordination of a tridentate ligand on the metallic center doesn't provoke any considerable changes on the formation of the C4 and C6, but the amount of C8 are decrease and the C10 and C12+ have increased. The Polymers produced by the catalyst 3a to 3 and 20 bar of ethylene have, according to analyses by DSC, the temperatures of fusion of 133,8 and 136ºC respectively. It indicates that in the two cases the production of high density polyethylene. The molar mass, gotten by GPC, is 46647 g/mols with MwD = 2,4 (3 bar). The system 3c/MAO showed values of TOF, activity and selectivity to different α-olefins according to the pressure of ethylene uses. Himself that shown a big sensibility to the concentration of ethylene solubilized.

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39

May, Masnou Anna. "Insights into nanomaterials: from surfactant systems to meso/macroporous materials and nanoparticles." Doctoral thesis, Universitat de Barcelona, 2014. http://hdl.handle.net/10803/285940.

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Nanomaterials have structured components with at least one dimension of less than 100 nm. Their novel properties stem from their nanoscale dimensions and increased relative surface area, and they have a wide range of applications in several key fields, including medicine. In this thesis we focus on meso- and meso/macroporous silica materials and nanoparticle. We examine how the properties of nanomaterials are influenced by the experimental conditions used in their synthesis. We then explore the possibility of tailoring such properties by varying the parameters in the process of manufacture. To this end we prepared a range of materials, including mesoporous silica, meso/macroporous silica, silica porous spheres and silica nanoparticles and studied their properties. We also examined the micellar solutions and emulsions that are used in the synthesis of these materials, their micellar and droplet size, the phase behavior of the surfactant systems involved in the synthesis, the stability and rheological behavior of the emulsions and the scale up parameters for their preparation at different scales. The synthesis and characterization techniques include rheology, optical microscopy, nitrogen adsorption-desorption, X-ray scattering (SAXS and XRD), transmission and scattering electron microscopy (TEM and SEM), dynamic light scattering (DLS), zeta potential and thromboelastography, among others. In the first study we examined water-in-oil emulsions with a liquid crystal phase as continuous phase. These systems are stable and highly elastic. Their microstructure is discussed by fitting the data with several rheological models. These systems are also compared with water-in-oil emulsions with a micellar phase in the continuous phase, and as a function of surfactant concentration and volume fraction of dispersed phase. In the second study, the process variables that have a significant effect on the properties of the emulsions are identified, including stirring rate, dispersed phase addition flow rate, surfactant concentration and scale up. Droplet size and rheological properties are considered as response variables. Stirring rate is the parameter that most influences the emulsion properties, followed by surfactant concentration. Vessel size is also important. To study the scale up, emulsions were prepared at three scales with geometric similarity and we identified the parameters that must be kept constant to obtain the same emulsion in the three scales, i.e. emulsions with the same droplet size, viscosity, yield stress, viscoelastic parameters and stability. The scale invariants take into account the stirring rate (N) and the scale (D, impeller diameter). The third study focuses on the preparation of meso and meso/macroporous materials. Bimodal mesoporous materials with an ordered hexagonal structure and two interconnected networks are prepared from a mixture of two surfactants, one hydrogenated and the other fluorinated, through the cooperative templating mechanism, using tetramethyl orthosilicate as silica source. The synthesis of ordered mesoporous materials from a novel surfactant consisting of a modified block copolymer with amino-groups on the ends (Jeffamine) is also studied. In this case, the best ordering of the mesopores is obtained at low temperature. In both studies, the surfactant phase behavior, and the structural properties of both surfactants and materials are determined, and the experimental conditions (pH, temperature, agitation) are optimized. Macroporous materials are then prepared from the oil-in-water emulsions stabilized with modified Jeffamine and using decane as organic phase, through the emulsion templating mechanism. Finally, mesoporous silica spheres are prepared from highly concentrated water-in-oil emulsions. The last study focuses on the synthesis and applications of silica nanoparticles. The process variables that have a direct effect on the size are identified, like the silica source concentration and the pH. The growth mechanism of these particles is studied through turbidimetry and explained in terms of nuclei formation and aggregation of the hydrolyzed species. The clotting properties of the particles are analyzed, in order to use these particles as a scaffold for further functionalization and application in the control of internal hemorrhages. First, the particles are functionalized to reduce the clotting activity, in order to avoid the formation of unwanted clots. Amino-functionalization and PEGylation are analyzed in this case. Second, functionalization with polyphosphate chains is studied in order to enhance the clotting activity, not only in normal conditions, but also under coagulopathy and hypothermia.
Els nanomaterials són materials amb propietats morfològiques entre 1 i 100 nm en almenys una direcció. En aquesta tesi s'estudien els materials meso- i meso/macroporosos de sílice, que tenen porus en aquestes dimensions, i nanopartícules, la grandària de les quals es troba també en aquest rang. En una primera fase s'estudien els sistemes tensioactius, com les solucions micel·lars i les emulsions, que s'usen per a la síntesi d’aquests materials. El primer estudi consta de l’anàlisi de les emulsions formades amb cristall líquid a la fase contínua. La microestructura d'aquests sistemes s'estudia amb diversos models reològics. També es comparen amb sistemes amb fase micel·lar en la fase contínua i a diferents concentracions de tensioactiu i fase dispersa. En un segon estudi es determinen les variables de procés que tenen un efecte significatiu sobre les propietats de les emulsions. Com a variables de resposta s'usen la mida de gota i les propietats reològiques. També s'estudia l'escalat en la preparació de les emulsions altament concentrades i es determinen els invariants d’escala. El tercer estudi se centra en la preparació de materials meso i meso/macroporosos. Es sintetitza un material amb mesoporus bimodals i estructura hexagonal ordenada a partir d'una barreja de dos tensioactius, i la síntesi de materials mesoporosos ordenats a partir d'uns tensioactius amb grups amino. També es preparen materials amb macroporus a partir d'emulsions formades amb aquest tensioactiu i, en última instància, es preparen esferes mesoporoses de sílice a partir d'emulsions aigua-en-oli altament concentrades. L'últim estudi se centra en la síntesi de nanopartícules de sílice, en les variables de procés que tenen un efecte directe sobre la mida obtinguda, i en l'aplicació d'aquestes nanopartícules en la coagulació de la sang per controlar hemorràgies internes. S'estudien les propietats de coagulació i es funcionalitzen amb agents que acceleren o disminueixen aquesta activitat. Les tècniques de síntesi i caracterització inclouen reologia, microscòpia òptica, adsorció-desorció de nitrogen, dispersió de raigs X, microscòpia electrònica de transmissió i de rastreig (TEM i SEM) i potencial zeta, entre altres.

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Elsherif, Ahmed Gamal Attallah Abdelmaksoud [Verfasser]. "Study of the pore systems of metal-organic frameworks, mesoporous silica, and low-k dielectric layers by means of positron annihilation spectroscopy / Ahmed Gamal Attallah Abdelmaksoud Elsherif." Halle, 2018. http://d-nb.info/1160514496/34.

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Ruhge, Forrest. "EFFECT OF GERMANIUM DOPING ON ERBIUM SENSITIZATION IN THE ERBIUM DOPED SILICON RICH SILICA MATERIAL SYSTEM." Master's thesis, University of Central Florida, 2006. http://digital.library.ucf.edu/cdm/ref/collection/ETD/id/2933.

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The continued size reduction in electronic integrated circuits has lead to a demand for on-chip high-bandwidth and low loss communication channels. Optical interconnects are considered an essential addition to the silicon electronics platform. A major challenge in the field of integrated Si photonics is the development of cost effective silicon compatible light sources. This thesis investigates the sensitization of group IV doped silica films emitting at 1.535μm for applications as silicon compatible light sources. Thin erbium-doped silica films containing excess silicon and germanium were deposited using a multi-gun sputter system. The composition of the deposited materials was verified by Rutherford Backscattering Spectrometry. Samples from each deposition were annealed in a controlled atmosphere tube furnace at temperatures between 500ºC and 1100ºC for 30 minutes. The photoluminescence spectra from the visible to the near-infrared region were acquired while pumping either near or far from the Er3+ absorption lines. Under both excitation conditions all samples annealed at temperatures below 1000ºC show clear emission at 1.535μm from Er3+ ions in the host material. In the current literature this is attributed to exciton mediated excitation of the Er3+. By contrast, in these studies indirect excitation was observed for samples annealed at temperatures well below the onset of nanocrystal nucleation and growth (between 500ºC and 1000ºC), suggesting excitation via small clusters or lattice defects. These findings could have significant implications in the further development of group IV sensitized silicon compatible gain media.
M.S.
Other
Optics and Photonics
Optics

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42

Kamapantula, Bhanu K. "In-silico Models for Capturing the Static and Dynamic Characteristics of Robustness within Complex Networks." VCU Scholars Compass, 2015. http://scholarscompass.vcu.edu/etd/4049.

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Understanding the role of structural patterns within complex networks is essential to establish the governing principles of such networks. Social networks, biological networks, technological networks etc. can be considered as complex networks where information processing and transport plays a central role. Complexity in these net works can be due to abstraction, scale, functionality and structure. Depending on the abstraction each of these can be categorized further. Gene regulatory networks are one such category of biological networks. Gene regulatory networks (GRNs) are assumed to be robust under internal and external perturbations. Network motifs such as feed-forward loop motif and bifan motif are believed to play a central role functionally in retaining GRN behavior under lossy conditions. While the role of static characteristics like average shortest path, density, degree centrality among other topological features is well documented by the research community, the structural role of motifs and their dynamic characteristics are not xiii well understood. Wireless sensor networks in the last decade were intensively studied using network simulators. Can we use in-silico experiments to understand biological network topologies better? Does the structure of these motifs have any role to play in ensuring robust information transport in such networks? How do their static and dynamic roles diﬀer? To understand these questions, we use in-silico network models to capture the dynamic characteristics of complex network topologies. Developing these models involve network mapping, sink selection strategies and identifying metrics to capture robust system behavior. Further, I studied the dynamic aspect of network characteristics using variation in network information ﬂow under perturbations deﬁned by lossy conditions and channel capacity. We use machine learning techniques to identify significant features that contribute to robust network performance. Our work demonstrates that although the structural role of feed-forward loop motif in signal transduction within GRNs is minimal, these motifs stand out under heavy perturbations.

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43

Cirillo, Silvia <1990&gt. "Personalization of Electronic Nicotine Delivery Systems Toxicological impact in in-vivo model." Doctoral thesis, Alma Mater Studiorum - Università di Bologna, 2020. http://amsdottorato.unibo.it/9182/1/Silvia%20Cirillo_Tesi.pdf.

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Electronic nicotine delivery systems (ENDS) use has recently grown. E-cig generates carcinogenic chemical compounds and reactive oxygen species (ROS). Carbonyls and ROS are formed when the liquid comes into contact with the heating element. In this study the chemical and biological effects of coil resistance applied on the same device were investigated. A preliminary in-vivo study the new heat-not-burn devices (IQOS®) has been conducted to evaluate the effect of the device on antioxidant biomarkers. The amount of formaldehyde, acetaldehyde, acrolein was measured by GC-MS analysis. The two e-liquids used for carbonyls detection differed only for the presence of nicotine. The nicotine-free liquid was then used for the detection of ROS in the aerosol. The impact of the non-nicotine vapor on cell viability in H1299 human lung carcinoma cells, as well as the biological effects in a rat model of e-cig aerosol exposure, were also evaluated. After the exposure of Sprague Dawley rats to e-cig and IQOS® aerosol, the effect of 28-day treatment was examined on enzymatic and non-enzymatic antioxidant response, lung inflammation, blood homeostasis and tissue damage by using scanning electron microscope (SEM) technique. The results show a significant correlation between the low resistance and the generation of higher concentrations of the selected carbonyls and ROS in aerosols. Cell viability was reduced with an inverse relation to coil resistance. The experimental model highlighted an impairment of the pulmonary antioxidant and detoxifying machinery. Frames from SEM show disorganization of alveolar and bronchial epithelium. IQOS® exposed animals shows a significant production of ROS related to the unbalance of antioxidant defense and alteration of macromolecule integrity. This research demonstrates how several toxicological aspects can potentially occur in e-cig consumers who use low resistance device coupled with nicotine-free liquid. ENDS may expose users to hazardous compounds, which, may promote chronic pathologies and degenerative diseases.

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Chen, Ming. "In silico systems analysis of biopathways." [S.l. : s.n.], 2004. http://deposit.ddb.de/cgi-bin/dokserv?idn=972067272.

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González, Fernández Alfredo A. "Studies and integration of Silicon-based light emitting systems." Doctoral thesis, Universitat de Barcelona, 2014. http://hdl.handle.net/10803/285863.

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This project presents the study of luminescent devices and materials based on silicon for its use in the fabrication of an optical system that integrates light emitter, waveguide, and light sensor in a single chip obtained by the use of standard CMOS techniques and materials. The atomic and structural characteristics of the materials are analysed and related to its luminescent response. Taking into account the results from the active material characterization, the design, fabrication, and characterization of electroluminescent devices based on such materials is presented. Finally, the design, fabrication and characterization of a complete CMOS compatible Integrated Optical System consisting of a transceiver, is discussed and analysed. The active materials used for light emission were different Silicon Rich Silicon Dioxide(SRO) and SRO-Si3 N4 bi-layers, obtained by a variety of CMOS compatible techniques and fabrication parameters. Two contributing mechanisms to photoluminescence in SRO were identified in all cases, respectively linked to the presence of radiative defects, and to Quantum Confinement phenomena. It is proposed and tested a model to describe the latter, based on the effective mass approximation, and the relation between the amount of Si-Si links and the volume of nano-agglomerates present in the material. In bi-layer samples, an additional luminescence band was observed, found to be generated in the transition material between silicon nitride and dioxide, and related to energy states introduced by defects. Samples with SRO thickness ten times higher than that of nitride, presented a clear dominance of the photoluminescence related to the dioxide. The centres responsible for electroluminescence in the electronicd evices were found to be fundamentally the same as those for photoluminescence despite the differences in measured spectra, and it was concluded that the influence of the architecture on the light output is of significant importance. It was shown that bi-layered devices delivered better results in terms of efficiency, light emission control, distribution and stability. The carrier transport mechanisms observed in the devices were dominated by material breakdown in single-layered devices, and Trap-assisted Tunnelling in the bi-layers. The Optical System integrating the light emitter, a waveguide, and a light detector, was designed and fabricated based on the results from the fabrication and analysis of the stand alone light emitting devices. During the design stage, it was corroborated by computer simulations that the characteristics of thelight emittedby thedevices thatpresented thehighest e.ciency and reliability, were suitable for its transmission trough the proposed waveguide architecture. The detection capabilities of the designed light sensors were also theoretically corroborated to be appropriated for the detection of the emitted light type. The proper functioning of the elements conforming the finally fabricated system was probed. Differences were found in the operation of the stand alone light emitting devices and those integrated, but the resulting luminescence was within the boundaries of the transmittable spectrum. The operation of the Integrated Optical System was tested and preliminarily studied, obtaining positive results in its stimulus-detection response, fulfilling the main objective of the work, and opening the door for further studies which can lead to the optimization of the design for particular applications.
Este proyecto aborda el estudio de dispositivos y materiales luminiscentes basados en silicio para su uso en la fabricación de un sistema óptico que integre emisor de luz, guía de ondas, y sensor en un solo chip obtenido mediante el uso de técnicas y materiales estándar para la fabricación CMOS. Las características atómicas y estructurales de los materiales son analizados y relacionados con su respuesta luminiscente. Considerando los resultados de la caracterización del material activo, se presenta el diseño, fabricación, y caracterización de dispositivos electroluminiscentes basados en dichos materiales. Finalmente, se discute y analizan el diseño, fabricación, y caracterización de un transceptor como Sistema Óptico Integrado. Los materiales activos para la emisión de luz fueron distintos Dióxidos de Silicio enriquecidos con Silicio (SRO por sus siglas en inglés) y bi-capas SRO-Si3 N4, obtenidos mediante una variedad de técnicas compatibles con los procesos CMOS y distintos parámetros para los mismos. Se identificaron dos mecanismos que contribuyen a la fotoluminiscencia del SRO en todos los casos, relacionados con defectos radiativos y fenómenos de Confinamiento Cuántico, respectivamente. Se sugiere y pone a prueba un modelo para describir este último, basado en la aproximación de la masa efectiva y la relación entre la cantidad de enlaces Si-Si y el volumen de nano-aglomerados. En muestras bi-capa, se observó una banda adicional de luminiscencia, cuya generación fue identificada en el material de transición entre el nitruro de silicio y el óxido, y relacionada con estados de energía introducidos por defectos. Muestras con un espesor de SRO diez veces mayores a aquel del nitruro presentaron una clara dominación de la luminiscencia relacionada con el óxido. Se halló que los centros responsables por la electroluminiscencia en los dispositivos electrónicos son fundamentalmente los mismos que los responsables de la fotoluminiscencia a pesar de las diferencias en los espectros medidos, y se concluyó que la influencia de la arquitectura sobre el espectro de salida es de importancia significativa. Se mostró que dispositivos bi-capa entregan mejores resultados en términos de eficiencia, control sobre la luz emitida, distribución de la misma, y estabilidad en el funcionamiento. Se observó que los mecanismos de transporte de carga hallados en los dispositivos están dominados por ruptura del material en el caso de dispositivos de una sola capa, y Tuneleo Asistido por Trampas en el caso de dispositivos bi-capa. El Sistema Óptico que integra el emisor, una guía de ondas, y el detector de luz, fue diseñado y fabricado con base en los resultados de la fabricación y análisis de los dispositivos emisores de luz aislados. Durante la etapa de diseño, se corroboró mediante simulaciones por computadora que las características de la luz emitida por los dispositivos que presentaron la máxima eficiencia y fiabilidad fueran apropiadas para su transmisión a través de la guía de ondas propuesta. También se corroboró teóricamente que las capacidades de detección de los sensores diseñados fuera la adecuada para el tipo de luz emitida. Se exploró el apropiado funcionamiento de los elementos del sistema finalmente fabricado. Se encontraron diferencias en la operación de los dispositivos emisores de luz aislados y aquellos integrados, pero la luminiscencia resultante se halló dentro de los límites del espectro transmisible. La operación del Sistema Óptico Integrado fue probada y estudiada de manera preliminar, con la obtención de resultados positivos en su respuesta estímulo-detección, cumpliendo así con el objetivo principal del trabajo, y abriendo la puerta para estudios posteriores que pueden guiar a la optimización del diseño del sistema para aplicaciones particulares.

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46

Griffin, N. "Low-dimensional systems in silicon/silicon-germanium heterostructures." Thesis, University of Cambridge, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.599710.

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Recent advances in epitaxial growth technology have made the formation of high-quality, strained-layer heterostructures in the silicon-germanium material system possible. This thesis presents an overview of a range of low-temperature measurements of some of these structures. As the materials are relatively new, the processing techniques for making samples are not well-established, so the thesis discusses the methods used, and in particular, it describes a variety of attempts to fabricate gated devices. Transport measurements of a high-mobility two-dimensional hole gas at low temperatures are described and analysed. Effective mass, quantum lifetime and phase-coherence times are extracted, with the temperature-dependence of the latter following a power-law, the exponent of which indicates a relatively clean system. This exponent predicts the scaling exponents around quantum Hall effect to Hall insulator transitions which are also measured. Screening is shown to cause a strong temperature-dependence of the conductivity. Transport measurements of ungated and Schottky-gated samples of high-quality two-dimensional electron gases at low temperatures are also presented. General features are discussed, including a strong overshoot associated with odd-numbered Hall plateaux and an accompanying asymmetry in the valley-spilt Shubnikov-de Haas peaks. A possible explanation in terms of strong inter-valley scattering is put forward. A range of new behaviours is shown to arise when the carrier density is varied by means of a gate. An anomalous quenching of the valley splitting at a filling factor of 3, resistivity fluctuations at high fields and other effects are presented and discussed. Finally, the thesis describes far infrared measurements of a range of electron gas samples. Cyclotron resonance frequencies of ungated samples deviated from the expected proportionality to the magnetic field. This is explained as resulting from a disorder potential coupled with electron-electron interactions, leading to an apparent lateral confinement.

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47

Largenton, Béatrice. "Etude rhéologique de systemes "chitosane-silice"." Brest, 1996. http://www.theses.fr/1996BRES2002.

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Dans ce travail, nous avons etudie le comportement rheologique de systemes chitosane-silice. Nous avons d'abord caracterise separement les solutions de chitosane et les suspensions de silice dans des conditions physico-chimiques identiques. Nous avons montre que le chitosane se comporte comme un polymere neutre possedant une certaine rigidite et adopte une conformation en pelote. Les particules de silice, quant a elles, forment des agregats tres aeres. Les particules de silice sont dispersees dans une solution de chitosane. L'adsorption des chaines de chitosane sur la surface de particules, mise en evidence dans cette etude, influence la stabilite des suspensions de silice et leurs proprietes rheologiques. A concentration fixe en polymere, la viscosite et les grandeurs viscoelastiques lineaires sont mesurees en fonction de la fraction volumique de silice. Les proprietes rheologiques ont ete reliees a la structure des systemes formes. Ainsi, pour une concentration en chitosane relativement faible, les agregats de silice sont stabilises steriquement par l'intermediaire de la couche de polymere adsorbee. Pour une concentration en polymere plus elevee (regime semi-dilue enchevetre), des amas d'agregats se forment le plus probablement par l'enchevetrement de chaines libres en solution avec les chaines adsorbees

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48

Sun, Chen Ph D. Massachusetts Institute of Technology. "Silicon-photonics for VLSI systems." Thesis, Massachusetts Institute of Technology, 2015. http://hdl.handle.net/1721.1/99784.

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Thesis: Ph. D., Massachusetts Institute of Technology, Department of Electrical Engineering and Computer Science, 2015.
This electronic version was submitted by the student author. The certified thesis is available in the Institute Archives and Special Collections.
Cataloged from student-submitted PDF version of thesis.
Includes bibliographical references (pages 173-183).
As raw compute power of a single chip continues to scale into the multi-teraflop regime, the processor I/O communication fabric must scale proportionally in order to prevent a performance bottleneck. As electrical wires suffer from high channel losses, pin-count constraints, and crosstalk, they are projected to fall short of the demands required by future memory systems. Silicon-photonic optical links overcome the fundamental tradeoffs of electrical wires; dense wavelength division multiplexing (DWDM) - where multiple data channels share a single waveguide or fiber to greatly extend bandwidth density - and the potential to combine at chip-scale with a very large scale integrated (VLSI) CMOS electrical chip make them a promising alternative for next-generation processor I/O. The key device for VLSI photonics is the optical microring resonator, a compact micrometer-scale device enabling energy-efficient modulation, DWDM channel selection, and sometimes even photo-detection. While these advantages have generated considerable interest in silicon-photonics, present-day integration efforts have been limited in scale owing to the difficulty of integration with advanced electronics and the sensitivity of microring resonators to both process and thermal variations. This thesis develops and demonstrates the pieces of a photonically-interconnected processor-to-memory system. We demonstrate a complete optical transceiver platform in a commercial 45 nm SOI process, showing that optical devices can be integrated into an advanced, commercial CMOS SOI process even without any changes to the manufacturing steps of the native process. To show that photonic interconnects are viable even for commoditized and cost-sensitive memory, we develop the first monolithic electronic-photonic links in bulk CMOS. As the stabilization of ring resonators is critical for use in VLSI systems, we contribute to the understanding of process and thermal variations on microring resonators, leading to the demonstration of a complete auto-locking microring tuning system that is agnostic to the transmitted data sequence and suitable for unencoded low-latency processor-to-memory traffic. Finally, the technology and methods developed in this work culminate in the demonstration of the world's first processor chip with integrated photonic interconnects, which uses monolithically integrated photonic devices to optically communicate to main memory.
by Chen Sun.
Ph. D.

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49

Lintereur, Phillip. "EFFECTS OF SOURCE WATER BLENDING FOLLOWING TREATMENT WITH SODIUM SILICATE AS A CORROSION INHIBITOR ON METAL RELEASE WITHIN A WAT." Doctoral diss., University of Central Florida, 2008. http://digital.library.ucf.edu/cdm/ref/collection/ETD/id/2967.

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A study was conducted to investigate and quantify the effects of corrosion inhibitors on metal release within a pilot distribution system while varying the source water. The pilot distribution system consisted of pre-existing facilities from Taylor et al (2005). Iron, copper, and lead release data were collected during four separate phases of operation. Each phase was characterized by the particular blend ratios used during the study. A blended source water represented a water that had been derived from a consistent proportion of three different source waters. These source waters included (1) surface water treated through enhanced coagulation/sedimentation/filtration, (2) conventionally treated groundwater, and (3) finished surface water treated using reverse osmosis membranes. The corrosion inhibitors used during the study were blended orthophosphate (BOP), orthophosphate (OP), zinc orthophosphate (ZOP), and sodium silicate (Si). This document was intended to cite the findings from the study associated with corrosion treatment using various doses of sodium silicate. The doses were maintained to 3, 6, and 12 mg/L as SiO2 above the blend-dependent background silica concentration. Sources of iron release within the pilot distribution system consisted of, in the following order of entry, (1) lined cast iron, (2) un-lined cast iron, and (3) galvanized steel. Iron release data from these materials was not collected for each individual iron source. Instead, iron release data represented the measurement of iron upon exposure to the pilot distribution system in general. There was little evidence to suggest that iron release was affected by sodium silicate. Statistical modeling of iron release suggested that iron release could be described by the water quality parameters of alkalinity, chlorides, and pH. The R2 statistic implied that the model could account for only 36% of the total variation within the iron release data set (i.e. R2 = 0.36). The model implies that increases in alkalinity and pH would be expected to decrease iron release on average, while an increase in chlorides would increase iron release. The surface composition of cast iron and galvanized steel coupons were analyzed using X-ray photoelectron spectroscopy (XPS). The surface analysis located binding energies consistent with Fe2O3, Fe3O4, and FeOOH for both cast iron and galvanized steel. Elemental scans detected the presence of silicon as amorphous silica; however, there was no significant difference between scans of coupons treated with sodium silicate and coupons simply exposed to the blended source water. The predominant form of zinc found on the galvanized steel coupons was ZnO. Thermodynamic modeling of the galvanized steel system suggested that zinc release was more appropriately described by Zn5(CO3)2(OH)6. The analysis of the copper release data set suggested that treatment with sodium silicate decreased copper release during the study. On average the low, medium, and high doses decreased copper release, when compared to the original blend source water prior to sodium silicate addition, by approximately 20%, 30%, and 50%, respectively. Statistical modeling found that alkalinity, chlorides, pH, and sodium silicate dose were significant variables (R2 = 0.68). The coefficients of the model implied that increases in pH and sodium silicate dose decreased copper release, while increases in alkalinity and chlorides increased copper release. XPS for copper coupons suggested that the scale composition consisted of Cu2O, CuO, and Cu(OH)2 for both the coupons treated with sodium silicate and those exposed to the blended source water. Analysis of the silicon elemental scan detected amorphous silica on 3/5 copper coupons exposed to sodium silicate. Silicon was not detected on any of the 8 control coupons. This suggested that sodium silicate inhibitor varied the surface composition of the copper scale. The XPS results seemed to be validated by the visual differences of the copper coupons exposed to sodium silicate. Copper coupons treated with sodium silicate developed a blue-green scale, while control coupons were reddish-brown. Thermodynamic modeling was unsuccessful in identifying a controlling solid that consisted of a silicate-based cupric solid. Lead release was generally decreased when treated with sodium silicate. Many of the observations were recorded below the detection limit (1 ppb as Pb) of the instrument used to measure the lead concentration of the samples during the study. The frequency of observations below the detection limit tended to increase as the dose of sodium silicate increased. An accurate quantification of the effect of sodium silicate was complicated by the observations recorded below detection limit. If the lead concentration of a sample was below detection limit, then the observation was recorded as 1 ppb. Statistical modeling suggested that temperature, alkalinity, chlorides, pH, and sodium silicate dose were important variables associated with lead release (R2 = 0.60). The exponents of the non-linear model implied that an increase in temperature, alkalinity, and chlorides increased lead release, while an increase in pH and sodium silicate dose were associated with a decrease in lead release. XPS surface characterization of lead coupons indicated the presence of PbO, PbO2, PbCO3, and Pb3(OH)2(CO3)2. XPS also found evidence of silicate scale formation. Thermodynamic modeling did not support the possibility of a silicate-based lead controlling solid. A solubility model assuming Pb3(OH)2(CO3)2 as the controlling solid was used to evaluate lead release data from samples in which lead coupons were incubated for long stagnation times. This thermodynamic model seemed to similarly describe the lead release of samples treated with sodium silicate and samples exposed to the blended source water. The pH of each sample was similar, thus sodium silicate, rather than the corresponding increase in pH, would appear to be responsible if a difference had been observed. During the overall study, the effects of BOP, OP, ZOP, and Si corrosion inhibitors were described by empirical models. Statistically, the model represented the expected value, or mean average, function. If these models are to be used to predict a dose for copper release, then the relationship between the expected value function and the 90th percentile must be approximated. The USEPA Lead and Copper Rule (LCR) regulates total copper release at an action level of 1.3 mg/L. This action level represents a 90th percentile rather than a mean average. Evaluation of the complete copper release data set suggested that the standard deviation was proportional to the mean average of a particular treatment. This relationship was estimated using a linear model. It was found that most of the copper data sub-sets (represented by a given phase, inhibitor, and dose) could be described by a normal distribution. The information obtained from the standard deviation analysis and the normality assumption validated the use of a z-score to relate the empirical models to the estimated 90th percentile observations. Since an analysis of the normality and variance (essentially contains the same information as the standard deviation) are required to assess the assumptions associated with an ANOVA, an ANOVA was performed to directly compare the effects of the inhibitors and corresponding doses. The findings suggested that phosphate-based inhibitors were consistently more effective than sodium silicate when comparing the same treatment levels (i.e. doses). Among the phosphate-based inhibitors, the effectiveness of each respective treatment level was inconsistent (i.e. there was no clear indication that any one phosphate-based inhibitor was more effective than the other). As the doses increased for each inhibitor, the results generally suggested that there was a corresponding tendency for copper release to decrease.
Ph.D.
Department of Civil and Environmental Engineering
Engineering and Computer Science
Electrical Engineering PhD

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50

Damart, Tanguy. "Energy dissipation in oxide glasses." Thesis, Lyon, 2017. http://www.theses.fr/2017LYSE1189/document.

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L'atténuation d'ondes à basse et haute fréquences dans les verres n'est pas encore bien comprise en grande partie car les phénomènes à l'origine de cette dissipation varient grandement en fonction de la fréquence. L’existence de structures complexes et organisation multi échelle dans les verres favorise l'apparition de temps de relaxation allant de la seconde à la femtoseconde et de corrélation prenant place de l’Angström à la centaine de nanomètre. A basse fréquence, une meilleur compréhension de ces phénomènes de dissipation serait bénéfique à de nombreux domaines. Par exemple, les multi-couches recouvrants les miroirs des interféromètres servant à détecter les ondes gravitationnelles sont réalisées à partir de verres d'oxyde (SiO2 et Ta2O5) qui sont une source majeur de dissipation. A haute fréquence, l'étude de la dissipation pose des questions théoriques sur le lien entre asymétrie locale et atténuation acoustique.Durant cette étude, nous avons réalisé une analyse approfondie de l'interaction entre ondes mécaniques et structure des verres en utilisant des techniques de simulations telle que la dynamique moléculaire. En partant de la synthèse de verres de SiO2 et Ta2O5, nous nous sommes appliqués à trouver l'origine structurelle de la dissipation aux différentes échelles de fréquence. A basse fréquence nous avons été capable de catégoriser les déplacements atomiques à l'origine de la dissipation en utilisant la théorie des états à deux niveaux. A haute fréquence, nous avons utilisé une technique de spectroscopie mécanique appuyé par un développement analytique pour montrer l'importance du désordre local dans l’existence de dissipation
The origin of sound attenuation at low and high frequency in glasses stays elusive mainly because of the complex temperature and frequency dependence of the phenomena at its root. Indeed, the presence of complex structures and multi-scale organizations in glasses induce the existence of relaxation time ranging from the second to the femto-second and of spatial correlation ranging from the Angström to a hundred nanometers. At low-frequency, a better understanding of the phenomena at the origin of dissipation would be beneficial to several applications. For example, the multi-layers coating the mirrors of gravitational waves detectors consists of a superposition of two oxide glasses: silicate (SiO2) and tantalum pentoxide (Ta2O5), are an important source of dissipation. At high frequency, the study of dissipation raises theoretical questions about the link between attenuation and dissipation as well as between loclt asymmetry and dissipation. In the present study, we conducted an analysis of the interaction between mechanical waves and the structure of two oxide glasses using simulation techniques such as non-equilibrium molecular dynamics. At high-frequencies, we implemented and used mechanical spectroscopy to measure dissipation numerically and performed in parallel an analytical development based on the projection of the atomic motion on the vibrational eigenmodes. At low-frequencies, we used molecular dynamics to gather sets of thermally activated events that we classed in three categories based on topologically distinct atomic motions and from which we predicted dissipation numerically using a refreshed TLS model

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