Thesis (M.S.)--West Virginia University, 2009. / Title from document title page. Document formatted into pages; contains xi, 71 p. : ill. (some col.). Includes abstract. Includes bibliographical references (p. 69-71).

Thesis (M.S.)--University of Texas at El Paso, 2009. / Title from title screen. Vita. CD-ROM. Includes bibliographical references. Also available online.

Thesis (Ph.D)--Polymer, Textile and Fiber Engineering, Georgia Institute of Technology, 2010. / Committee Chair: Jacob. Karl; Committee Member: Griffin. Anselm; Committee Member: Tannenbaum. Rina; Committee Member: Thio. Yonathan S; Committee Member: Yao. Donggang. Part of the SMARTech Electronic Thesis and Dissertation Collection.

Thesis (Ph.D)--Chemistry and Biochemistry, Georgia Institute of Technology, 2009. / Committee Chair: Perry, Joseph W.; Committee Member: Kippelen, Bernard; Committee Member: Lyon, L. Andrew; Committee Member: Marder, Seth R.; Committee Member: Whetten, Robert L. Part of the SMARTech Electronic Thesis and Dissertation Collection.

Στην παρούσα πτυχιακή εργασία παρασκευάστηκαν νανοσύνθετα υλικά διοξειδίου του τιτανίου (TiO2)/παλυγορσκίτη (60:40, 70:30, 80:20) για την περιγραφή και μελέτη των χαρακτηριστικών τους ώστε να την εφαρμοστούν σε επόμενο στάδιο στη φωτοκαταλυτική αποδόμηση αέριοων ρύπων (των οξειδίων του αζώτου - NOx) και οι οργανικών πτητικών ενώσεων (VOC’s). Ο παλυγορσκίτης που χρησιμοποιήθηκε για την διεξαγωγή των πειραμάτων συλλέχτηκε από την λεκάνη του Βεντζίου στα Γρεβενά. Τα νανοσύνθετα παρασκευάστηκαν με τη μέθοδο διασποράς-επικάθησης του TiO2 και στις μικροΐνες του Παλυγορσκίτη. Η κρυσταλλική μορφή του TiO2 που συντέθηκε ήταν ο ανατάσης. Για τον χαρακτηρισμό των ιδιοτήτων των τροποποιημένων δειγμάτων εφαρμόστηκαν διαφορετικές τεχνικές όπως: περιθλασιμετρία ακτίνων X, υπέρυθρη φασματοσκοπία μετασχηματισμού κατά Fourier, ηλεκτρονική μικροσκοπία σάρωσης, ηλεκτρονική μικροσκοπία διερχόμενης δέσμης και προσδιορισμός μεγέθους και κατανομής πόρων καθώς και ειδικής επιφάνειας. Με την άυξηση του TiO2 στα δείγματα μας το αποτιθέμενο υλικό που είναι μεταξύ 3-10nm έδειξε ότι διασπίρεται σε όλη την επιφάνεια του παλυγορσκίτη. Επίσης τα τροποποιημένα με ΤιΟ2 δείγματά μας παρουσίασαν τη δημιουργία μεσοπορώδους δομής με πόρους μεγέθους κυρίως 5,8nm. Τα νανοσύνθετα εμφανίζουν ιδιότητες που φαίνεται να τα καθιστούν αρκετά αποτελεσματικά για τη εφαρμογή τους στους αέριους ρύπους NOx και ως εκ τούτου μπορούν να χρησιμοποιηθούν και για άλλους αέριου ρύπους όπως οι οργανικές πτητικές ενώσεις VOC’s. / In this study three TiO2-Pal nanocomposites were prepared (80:20, 70:30, 60:40). The synthesis and characterization of the nanocomposite were conducted in order to be applied (in a next stage) in several environmental applications including the photocatalytic degradation of Nitrogen oxides (NOx) and volatile organic compounds (VOC’s). The palygorskite sample was collected from Western Macedonia (Grevena, Ventzia basin). The samples were prepared by dispersing TiO2 nanoparticles on the microfibers of palygorskite. The crystal form of TiO2 that was synthesized was anatase. The physical properties of the nanocomposites were tested using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), attenuated total reflection using Fourier transform infrared spectroscopy (ATR-FTIR) and N2 surface analysis by BET. By increasing the amount of the TiO2 in the nanocomposites, the deposited 3-10nm TiO2 particles were found to be aggregated on the surfaces of the palygorskite particles. After treating with TiO2, the nanocomposites showed largely interpaticle mesopores of about 5.8nm. The properties of nanocomposites that were measured are very promising showing that all three of them could be effective photocatalysts in decomposing air pollutants like NOx and probably other air pollutants such as volatile organic compounds (VOC’s).

Submitted by Maria Medeiros (maria.dilva1@ufcg.edu.br) on 2018-09-12T12:56:27Z No. of bitstreams: 1 DANIELA DE LOURDES ANJOS COUTINHO SIMÕES ANDRADE - TESE (PPGEP) 2009.pdf: 2248344 bytes, checksum: 28a93ae4236853f59fe35037c2ab6f28 (MD5) / Made available in DSpace on 2018-09-12T12:56:27Z (GMT). No. of bitstreams: 1 DANIELA DE LOURDES ANJOS COUTINHO SIMÕES ANDRADE - TESE (PPGEP) 2009.pdf: 2248344 bytes, checksum: 28a93ae4236853f59fe35037c2ab6f28 (MD5) Previous issue date: 2009 / A proposta deste trabalho foi preparar nanocompósitos de polipropileno/compatibilizante/bentonita, pelo método de intercalação na fusão, utilizando como carga uma argila sódica comercial Argel, fornecida por uma indústria local, purificada e modificada organicamente com um sal quaternário de amônio empregando diferentes métodos de preparação. Ao longo do trabalho foram utilizadas duas matrizes e dois tipos de compatibilizantes: PP H103, PP H401, Polipropileno modificado com anidrido maleico (PP-g-MA) e Copolímero de etileno e álcool vinílico (EVOH), respectivamente. As argilas foram caracterizadas por difração de raios-X (DRX), espectroscopia de infravermelho (FTIR) e análise termogravimétrica (TG) visando determinar o método de preparação mais eficiente para obtenção das argilas organofílicas. Uma vez determinado o melhor procedimento para organofilização, na segunda parte deste estudo, avaliou-se o efeito do tipo e teor de argila organofílica, bem como o tipo e teor de compatibilizante nas propriedades de filmes de polipropileno. De acordo com os resultados preliminares deste estudo, há uma indicação de que os filmes de nanocompósitos PP/PP-g-MA/argila organofílica, contendo 1% de argila organofílica e 15% de polipropileno modificado com anidrido maléico (PP-g-MA) podem ser promissores para o mercado de embalagens e poderão em um futuro próximo serem usados como um novo produto por empresas nacionais. / The purpose of this work is to prepare nanocomposites of polypropylene/compatibilizer/bentonite, by melting intercalation, with a commercial sodium clay – Argel – as filler. This clay was organically purified and modified by different methods, with a quaternary ammonium salt. The clays were characterized by X-Ray diffraction (XRD), infrared spectroscopy (FTIR) and thermogravimetric analyses (TG) to determine the most efficient preparation method. Before that, in the second stage of this study, the influence of the type and contend of organoclay in the properties of the polypropylene films was measured; the same was done for the compatibilizer. The preliminary results indicate that the nanocomposites film with 1% of organoclay and 15% of polypropylene grafted with maleic anhydride show promise as packing materials and may be used, in the near future, as a new product by the national industry.

It is believed, that due to the large surface areas provided by the nano scale materials, various composite properties could be enhanced when such particles are incorporated into a polymer matrix. There is also a trend of utilizing natural resources or reusing and recycling materials that are already available for the fabrication of the new composite materials. Cellulose is the most abundant natural polymer on the planet, and therefore it is not surprising to be of interest for composite fabrication. Basic structures of cellulose, comprised of long polysaccharide chains, are the building blocks of cellulose nano fibers. Nano fibers are further bound into micro fibrils and macro fibers. Theoretically pure cellulose nano fibers have tremendous strengths, and therefore are some of the most sought after nano particles. The fiber extraction however is a complex task. The ultrasound, which creates pressure variation in the medium, was employed to extract nano-size cellulose particles from microcrystalline cellulose (MCC). The length and the intensity of the cavitations were evaluated. Electron microscopy studies revealed that cellulose nanoparticles were successfully obtained from the MCC after ultrasound treatment of just 30 minutes. Structure of the fractionated cellulose was also analyzed with the help of X-ray diffraction, and its thermal properties were evaluated with the help of differential scanning calorimetry (DSC). Ultrasound treatment performed on the wheat straw, kenaf, and miscanthus particles altered fiber structure as a result of the cavitation. The micro fibers were generated from these materials after they were subjected to NaOH treatment followed by the ultrasound processing. The potential of larger than nano-sized natural fibers to be used for composite fabrication was also explored. The agricultural byproducts, such as wheat or rice straw, as well as other fast growing crops as miscanthus or kenaf, are comprised of three basic polymers. Just like in wood the polymers are: cellulose, hemicelluloses, and lignin. When subjected to elevated pressures and temperatures, we are able to get access to some of these natural polymers and use them as a matrix material for composite fabrication. Therefore, fabrication of composite materials without addition of synthetic polymers is possible. Thermal and mechanical properties of such composites are evaluated with the help of electron microscopy, differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), thermogravimetric analysis (TGA), and flexural strength measurements. The chemical changes in the composites are also probed with the help of Fourier transform infrared (FTIR) analysis. Various additives introduced into composite materials provide different properties. The addition of small amounts of synthetic polymers further enhances the properties of natural fiber composites and do not require high fabrication pressures. Calcium sulfite crystals, which are one of the coal combustion products, were combined with the natural fibers and recycled HDPE polymer to form wood substitute composites. The introduction of these additives resulted in composites with the properties similar to those of the natural wood. Coal combustion products, often used in composite material fabrication, contain mercury which may be rereleased during composite fabrication. Mercury behavior under composite fabrication conditions, such as elevated pressures and temperatures were evaluated. Sulfite rich scrubber material, generated during the flue gas desulphurization process was the main target of the study. It was observed that the release of the mercury is highly dependent on the composite fabrication pressure as well as the temperature.

In this tribological study, a temperature dependent inquiry of the changes in chemistry and crystal structure of two selected double metal oxides is undertaken. It is known that chameleon coatings of Mo2N/Ag/MoS2 produce a friction coefficient of 0.1 from wear testing at 600 °C for 300,000 cycles. The low friction is attributed to the formation of silver molybdates layers, a lubricious double-metal oxide, in the coating. Double-metal oxides consisting of a group 6 transitional metal and silver (silver molybdate (Ag2Mo2O7) and silver tungstate (Ag2WO4)) were used for this investigation. Thin films and powders were investigated using high temperature x-ray diffraction, high-temperature Raman spectroscopy and differential scanning calorimetry in tandem with sliding tests from 25 to 600 °C. Our results were compared to external ab-initio molecular dynamic simulations performed elsewhere to qualify experimental results. The layered atomic structure of silver molybdate facilitates sliding, resulting in a low coefficient of friction (<0.2) from 300-500 °C. Unlike Ag2Mo2O7, however, Ag2WO4 does not possess a layered atomic structure and produced coefficients of friction (>0.4) in all temperature ranges between room temperature and 500 °C. Applying the knowledge gained from prior studies of the intrinsic properties of double metal oxides of group 6, chameleon coatings consisting of group 5 transitional metal nitrides (vanadium nitride, niobium nitride, and tantalum nitride) with silver inclusions were created using unbalanced magnetron sputtering to investigate their potential application as adaptive, friction reducing coatings. The coatings were tribotested against a Si3N4 counterface in the 22 to 1000 °C temperature range. In-situ Raman Spectroscopy measurements were taken during heating and wear testing at 700 °C to identify the evolution of phases in the coatings' surfaces and in the wear track. The chemical and structural properties of the coatings were also characterized before and after wear testing using x-ray diffraction. At higher temperatures, oxygen, silver and the transition metals react on the surface to form potentially lubricious double oxide phases (silver vanadate, silver niobate and silver tantalate). All coatings performed similarly up to 750 °C. The VN/Ag coating, however, had a lower coefficient of friction at 750 °C comparatively to TaN/Ag and NbN/Ag, likely due to its reported lower melting temperature (450 °C) and its layered crystal structure.

Master of Science / Department of Grain Science and Industry / Sajid Alavi / There is a renewed focus on biodegradable polymers in packaging applications due to environmental concerns associated with conventional plastics. Melt extrusion was used to synthesize nanocomposites from poly (lactic acid) (PLA) or poly (butylene succinate) (PBS) blended with natural nanofillers — chitin whiskers (CHW, 1-5%), nanocrystalline cellulose (NCC, 1-5%) or lignin-coated nanocrystalline cellulose (LNCC, 3%). Transmission electron microscopy and x-ray diffraction indicated that the natural nanofillers were uniformly dispersed in the polymer matrix. For PLA based nanocomposites, differential scanning calorimetry showed a decrease in change of heat capacity at glass transition (ΔCp) with increased nanofiller addition, indicating greater confinement of polymer chains. For PBS based nanocomposites, nanofillers acted as nucleating agents and promoted recrystallization of polymer as reflected in increase of degree of crystallinity (Xc) from 65.9-66.8 to 75.6%. By addition of NCC and CHW, tensile strength (TS) of PLA based films increased from 50.2 MPa to 70.9 MPa and 52.1 MPa, respectively, while TS of PBS increased from 23.2-24.9 MPa to 32.9 MPa and 43.6 MPa, respectively. Elongation at break (E%) of nanocomposite films ranged from 9.1 to 15.3, and in general decreased with addition of nanofillers. LNCC did not significantly improve mechanical properties of PBS and PLA films. Additionally, 3% NCC addition reduced oxygen transmission rate (OTR) of PLA from 209.9 to 180.8 cc/m[superscript]2/day, which further reduced to 109.3 cc/m[superscript]2/day by adding compatibilizer methylene diphenyl diisocyanate (MDI, 4%). Water vapor transmission rate (WVTR) of PLA also reduced from 44.4 to 28.6 g/m[superscript]2/day with 3% NCC and 4% MDI addition. Similarly OTR and WVTR of PBS decreased from 737.7 to 280 cc/m[superscript]2/day and 83.8 to 49.4 g/m[superscript]2/day, respectively with 3% NCC. Use of 4% MDI further reduced OTR and WVTR to 23.8 cc/m[superscript]2/day and 30.8 g/m[superscript]2/day, respectively. Use of starch can potentially reduce the costs of bio-based nanocomposites films. Up to 40% starch was incorporated during synthesis of PLA and NCC nanocomposites using solution mixing method. Addition of starch decreased TS from 35.8 MPa to 18.4 MPa and E% from 8.3% to 6.0%. Use of NCC (1%) and MDI (4%) improved the mechanical properties to a certain extent.

A presente dissertação tem por objetivo apresentar um estudo quanto à influência da adição de nanocargas nas proprie!dades térmicas, morfológicas, físicas e anticorrosivas de tintas em pó base resina epóxi. Nanocompósitos poliméricos aplicados a tinta em pó com teores de 2 e 4 % de montmorilonita organofílica (OMMT) (p/p) foram obtidos no estado ·fundido em extrusora dupla-rosca co-rotante, em diferentes velocidades de processamento. As tintas em pó foram aplicadas em substratos de aço-carbono por pulverização eletrostática. Os resu ltados obtidos demonstram que os parâmetros utilizados para a cura em estufa (200 °C por 1 O minutos) das tintas foram satisfatórios, não sendo observados picos exotérmicos nos termogramas de calorimetria exploratória diferencial (DSC). As análises térmicas demonstraram que a incorporação de OMMT resultou no aumento da temperatura de máxima degradação para as amostras antes da cura, e apresentou pouca influência nos revestimentos após a cura, apresentando ainda redução da reatividade (b.Hreação) das tintas em pó base epóxi com o aumento da velocidade de processamento, de 200 para 400 rpm. As análises morfológicas de difração de raios X (DRX) e microscopia eletrônica de transmissão (MET) indicaram a presença de estruturas com predominância esfoliada para os nanocompósitos, com boa dispersão da OMMT na matriz epóxi. A incorporação dos teores de 2 % (p/p) de OMMT, para ambas as velocidades de! processamento, resultou em revestimentos com melhores propriedades de resistência ao impacto, resistência a flexibil idade e de brilho. Os revestimentos obtidos com teores de 4 % de OMMT (p/p) apresentarem melhor desempenho quanto às propri1edades térmicas e resistência a corrosão, conforme análises de TGA e de exposição à névoa salina, respectivamente. As medidas de migração subcutânea realizadas após o ensaio de exposição à névoa salina indicaram revestimentos com melhores propriedades de barreira para as amostras com OMMT, corroborado pelos resultados de espectroscopia de impedância eletroquímica (ElE). / Submitted by Ana Guimarães Pereira (agpereir@ucs.br) on 2015-10-07T13:01:23Z No. of bitstreams: 1 Dissertacao Diego Piazza.pdf: 24298065 bytes, checksum: ceb0efa8d78e26b1bbd45581c9a739fe (MD5) / Made available in DSpace on 2015-10-07T13:01:23Z (GMT). No. of bitstreams: 1 Dissertacao Diego Piazza.pdf: 24298065 bytes, checksum: ceb0efa8d78e26b1bbd45581c9a739fe (MD5) / Conselho Nacional de Desenvolvimento Científico e Tecnológico, CNPq / The objective of this dissertation is to present a study of the influence of the addition of nanoclays on thermal, morphological, physical and anticorrosive properties of powder coatings epoxy resin based. Polymeric nanocomposites applied of powder coatings with leveis of 2 and 4 % of orgianophilic montmorillonite (OMMT) (w/w) were obtained in the melt state in extruder twin-screw co-rotation at different processing speeds. The powder coatings were applied to carbon steel substrates by electrostatic spraying. The results show that the parameters used for curing (200 °C for 10 minutes) the coatings were satisfactory, exothermic peaks were not observed in thermograms of differential scanning calorimetry (DSC). Thermal analysis showed that the incorporation of OMMT resulted in increasing the temperature of degradation maximum for the samples before curinn, and little influence in coatings after curing, also reduces the reactivity (~H reaction) of powder coatings based epoxy with increasing processing speed (400 rpm). The morphological analysis of X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated the presence of predominantly exfoliated structures for the nanocomposites, with good dispersion of OMMT in the epoxy matrix. The incorporation of th~e leveis of 2 % of OMMT (w/w), for both processing speed, resulted in coatings with improved impact strength, endurance, flexibility and gloss. The coatings obtained with leveis of 4 % of OMMT (w/w) having better performance on the thermal proiPerties and corrosion resistance, as thermal analysis and exposure to salt spray, respectively. Measures of subcutaneous migration made after salt spray teslting indicated coatings with better barrier properties for samples with OMMT, with was corroborated by electrochemical impedance spectroscopy (EIS) results.