Search results for: nano-micro crystalline diamond coating

Authors: Mercedes Bertotto, Marcelo Bello, Hector Goicoechea, Veronica Fusca

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The National Service of Agri-Food Health and Quality (SENASA), controls honey to detect contamination by synthetic or natural chemical substances and establishes and controls the traceability of the product. The utility of near-infrared spectroscopy for the detection of adulteration of honey with high fructose corn syrup (HFCS) was investigated. First of all, a mixture of different authentic artisanal Argentinian honey was prepared to cover as much heterogeneity as possible. Then, mixtures were prepared by adding different concentrations of high fructose corn syrup (HFCS) to samples of the honey pool. 237 samples were used, 108 of them were authentic honey and 129 samples corresponded to honey adulterated with HFCS between 1 and 10%. They were stored unrefrigerated from time of production until scanning and were not filtered after receipt in the laboratory. Immediately prior to spectral collection, honey was incubated at 40°C overnight to dissolve any crystalline material, manually stirred to achieve homogeneity and adjusted to a standard solids content (70° Brix) with distilled water. Adulterant solutions were also adjusted to 70° Brix. Samples were measured by NIR spectroscopy in the range of 650 to 7000 cm⁻¹. The technique of specular reflectance was used, with a lens aperture range of 150 mm. Pretreatment of the spectra was performed by Standard Normal Variate (SNV). The ant colony optimization genetic algorithm sample selection (ACOGASS) graphical interface was used, using MATLAB version 5.3, to select the variables with the greatest discriminating power. The data set was divided into a validation set and a calibration set, using the Kennard-Stone (KS) algorithm. A combined method of Potential Functions (PF) was chosen together with Partial Least Square Linear Discriminant Analysis (PLS-DA). Different estimators of the predictive capacity of the model were compared, which were obtained using a decreasing number of groups, which implies more demanding validation conditions. The optimal number of latent variables was selected as the number associated with the minimum error and the smallest number of unassigned samples. Once the optimal number of latent variables was defined, we proceeded to apply the model to the training samples. With the calibrated model for the training samples, we proceeded to study the validation samples. The calibrated model that combines the potential function methods and PLSDA can be considered reliable and stable since its performance in future samples is expected to be comparable to that achieved for the training samples. By use of Potential Functions (PF) and Partial Least Square Linear Discriminant Analysis (PLS-DA) classification, authentic honey and honey adulterated with HFCS could be identified with a correct classification rate of 97.9%. The results showed that NIR in combination with the PT and PLS-DS methods can be a simple, fast and low-cost technique for the detection of HFCS in honey with high sensitivity and power of discrimination.

Keywords: adulteration, multivariate analysis, potential functions, regression

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Authors: Supriya Majumder, Pabitra Banik

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Fates of Arsenic (As) on the soil-plant environment belong to the critical emerging issue, which in turn to appraises the threatening implications of a human health risk — assessing the dynamics of As in soil solid components are likely to impose its potential availability towards plant uptake. In the present context, we introduced an improved Sequential Extraction Procedure (SEP) questioning to identify solid-phase speciation of As in paddy soil under variable soil environmental conditions during two consecutive seasons of rice cultivation practices. We coupled gradients of water management practices with the addition of fertilizer amendments to assess the changes in a partition of As through a field experimental study during monsoon and post-monsoon season using two rice cultivars. Water management regimes were varied based on the methods of cultivation of rice by Conventional (waterlogged) vis-a-vis System of Rice Intensification-SRI (saturated). Fertilizer amendment through the nutrient treatment of absolute control, NPK-RD, NPK-RD + Calcium silicate, NPK-RD + Ferrous sulfate, Farmyard manure (FYM), FYM + Calcium silicate, FYM + Ferrous sulfate, Vermicompost (VC), VC + Calcium silicate, VC + Ferrous sulfate were selected to construct the study. After harvest, soil samples were sequentially extracted to estimate partition of As among the different fractions such as: exchangeable (F1), specifically sorbed (F2), As bound to amorphous Fe oxides (F3), crystalline Fe oxides (F4), organic matter (F5) and residual phase (F6). Results showed that the major proportions of As were found in F3, F4 and F6, whereas F1 exhibited the lowest proportion of total soil As. Among the nutrient treatment mediated changes on As fractions, the application of organic manure and ferrous sulfate were significantly found to restrict the release of As from exchangeable phase. Meanwhile, conventional practice produced much higher release of As from F1 as compared to SRI, which may substantially increase the environmental risk. In contrast, SRI practice was found to retain a significantly higher proportion of As in F2, F3, and F4 phase resulting restricted mobilization of As. This was critically reflected towards rice grain As bioavailability where the reduction in grain As concentration of 33% and 55% in SRI concerning conventional treatment (p <0.05) during monsoon and post-monsoon season respectively. Also, prediction assay for rice grain As bioavailability based on the linear regression model was performed. Results demonstrated that rice grain As concentration was positively correlated with As concentration in F1 and negatively correlated with F2, F3, and F4 with a satisfactory level of variation being explained (p <0.001). Finally, we conclude that F1, F2, F3 and F4 are the major soil. As fractions critically may govern the potential availability of As in soil and suggest that rice cultivation with the SRI treatment is particularly at less risk of As availability in soil. Such exhaustive information may be useful for adopting certain management practices for rice grown in contaminated soil concerning to the environmental issues in particular.

Keywords: arsenic, fractionation, paddy soil, potential availability

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Authors: Rideci Farias, Haroldo Paranhos

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The present work deals with the use of drainage geo-composite as a deep drainage and geogrid element to reinforce the base of the body of the landfill destined to the road pavement on geological faults in the stretch of the TO-342 Highway, between the cities of Miracema and Miranorte, in the State of Tocantins / TO, Brazil, which for many years was the main link between TO-010 and BR-153, after the city of Palmas, also in the state of Tocantins / TO, Brazil. For this application, geotechnical and geological studies were carried out by means of SPT percussion drilling, drilling and rotary drilling, to understand the problem, identifying the type of faults, filling material and the definition of the water table. According to the geological and geotechnical studies carried out, the area where the route was defined, passes through a zone of longitudinal fault to the runway, with strong breaking / fracturing, with presence of voids, intense alteration and with advanced argilization of the rock and with the filling up parts of the faults by organic and compressible soils leachate from other horizons. This geology presents as a geotechnical aggravating agent a medium of high hydraulic load and very low resistance to penetration. For more than 20 years, the region presented constant excessive deformations in the upper layers of the pavement, which after routine services of regularization, reconformation, re-compaction of the layers and application of the asphalt coating. The faults were quickly propagated to the surface of the asphalt pavement, generating a longitudinal shear, forming steps (unevenness), close to 40 cm, causing numerous accidents and discomfort to the drivers, since the geometric positioning was in a horizontal curve. Several projects were presented to the region's highway department to solve the problem. Due to the need for partial closure of the runway, the short time for execution, the use of geosynthetics was proposed and the most adequate solution for the problem was taken into account the movement of existing geological faults and the position of the water level in relation to several Layers of pavement and failure. In order to avoid any flow of water in the body of the landfill and in the filling material of the faults, a drainage curtain solution was used, carried out at 4.0 meters depth, with drainage geo-composite and as reinforcement element and inhibitor of the possible A geogrid of 200 kN / m of resistance was inserted at the base of the reconstituted landfill. Recent evaluations, after 13 years of application of the solution, show the efficiency of the technique used, supported by the geotechnical studies carried out in the area.

Keywords: geosynthetics, geocomposite, geogrid, road, recovery, geological failure

Procedia PDF Downloads 150

Authors: Leslie Raphael de M. Ferraz, Salvana Priscylla M. Costa, Tarcyla de A. Gomes, Giovanna Christinne R. M. Schver, Cristóvão R. da Silva, Magaly Andreza M. de Lyra, Danilo Augusto F. Fontes, Larissa A. Rolim, Amanda Carla Q. M. Vieira, Miracy M. de Albuquerque, Pedro J. Rolim-Neto

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Efavirenz (EFV) is a drug used as first-line treatment of AIDS. However, it has poor aqueous solubility and wettability, presenting problems in the gastrointestinal tract absorption and bioavailability. One of the most promising strategies to improve the solubility is the use of solid dispersions (SD). Therefore, this study aimed to characterize SD EFZ with the polymers: PVP-K30, PVPVA 64 and SOLUPLUS in order to find an optimal formulation to compose a future pharmaceutical product for AIDS therapy. Initially, Physical Mixtures (PM) and SD with the polymers were obtained containing 10, 20, 50 and 80% of drug (w/w) by the solvent method. The best formulation obtained between the SD was selected by in vitro dissolution test. Finally, the drug-carrier system chosen, in all ratios obtained, were analyzed by the following techniques: Differential Scanning Calorimetry (DSC), polarization microscopy, Scanning Electron Microscopy (SEM) and spectrophotometry of absorption in the region of infrared (IR). From the dissolution profiles of EFV, PM and SD, the values of area Under The Curve (AUC) were calculated. The data showed that the AUC of all PM is greater than the isolated EFV, this result is derived from the hydrophilic properties of the polymers thus favoring a decrease in surface tension between the drug and the dissolution medium. In adittion, this ensures an increasing of wettability of the drug. In parallel, it was found that SD whom had higher AUC values, were those who have the greatest amount of polymer (with only 10% drug). As the amount of drug increases, it was noticed that these results either decrease or are statistically similar. The AUC values of the SD using the three different polymers, followed this decreasing order: SD PVPVA 64-EFV 10% > SD PVP-K30-EFV 10% > SD Soluplus®-EFV 10%. The DSC curves of SD’s did not show the characteristic endothermic event of drug melt process, suggesting that the EFV was converted to its amorphous state. The analysis of polarized light microscopy showed significant birefringence of the PM’s, but this was not observed in films of SD’s, thus suggesting the conversion of the drug from the crystalline to the amorphous state. In electron micrographs of all PM, independently of the percentage of the drug, the crystal structure of EFV was clearly detectable. Moreover, electron micrographs of the SD with the two polymers in different ratios investigated, we observed the presence of particles with irregular size and morphology, also occurring an extensive change in the appearance of the polymer, not being possible to differentiate the two components. IR spectra of PM corresponds to the overlapping of polymer and EFV bands indicating thereby that there is no interaction between them, unlike the spectra of all SD that showed complete disappearance of the band related to the axial deformation of the NH group of EFV. Therefore, this study was able to obtain a suitable formulation to overcome the solubility limitations of the EFV, since SD PVPVA 64-EFZ 10% was chosen as the best system in delay crystallization of the prototype, reaching higher levels of super saturation.

Keywords: characterization, dissolution, Efavirenz, solid dispersions

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Authors: Gheorghiţa Mitran, Adriana Urdă, Mihaela Florea, Octavian Dumitru Pavel, Florentina Neaţu

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Oxidative dehydrogenation and hydrogenation reactions of L-malic acid are interesting ways for its transformation into valuable products, including oxaloacetic, pyruvic and malonic acids but also 1,4-butanediol and 1,2,4-butanetriol. Keto acids have a range of applicationsin many chemical syntheses as pharmaceuticals, food additives and cosmetics. 3-Hydroxybutyrolactone and 1,2,4-butanetriol are used for the synthesis of chiral pharmaceuticals and other fine chemicals, while 1,4-butanediol can be used for organic syntheses, such as polybutylene succinate (PBS), polybutylene terephthalate (PBT), and for production of tetrahydrofuran (THF). L-malic acid is a non-toxic and natural organic acid present in fruits, and it is the main component of wine alongside tartaric acid representing about 90% of the wine total acidity. Iron oxides dopped with cobalt (CoxFe3-xO4; x= 0; 0.05; 0.1; 0.15) were studied as catalysts in these reactions. There is no mention in the literature of non-noble transition metal catalysts for these reactions. The method used for catalysts preparation was coprecipitation, whileBET XRD, XPS, FTIR and UV-VIS spectroscopy were used for the physicochemical properties evaluation.TheXRD patterns revealed the presence of α-Fe2O3 rhombohedral hematite structure, with cobalt atoms well dispersed and embedded in this structure. The studied samples are highly crystalline, with a crystallite size ranged from 58 to 65 nm. The optical absorption properties were investigated using UV-Vis spectroscopy, emphasizing the presence of bands that correspond with the reported hematite nanoparticle. Likewise, the presence of bands corresponding to lattice vibration of hexagonal hematite structurehas been evidenced in DRIFT spectra. Oxidative dehydrogenation of malic acid was studied using as solvents for malic acid ethanol or water(2, 5 and 10% malic acid in 5 mL solvent)at room temperature, while the hydrogenation reaction was evaluated in water as solvent (5%), in the presence of 1% catalyst. The oxidation of malic acid into oxaloacetic acid is the first step, after that, oxaloacetic acid is rapidly decarboxylated to malonic acid or pyruvic acid, depending on the active site. The concentration of malic acid in solution, it, in turn, has an influence on conversionthis decreases when the concentration of malic acid in the solution is high. The spent catalysts after the oxidative dehydrogenation of malic acid in ethanol were characterized by DRIFT spectroscopy and the presence of oxaloacetic, pyruvic and malonicacids, along with unreacted malic acidwere observed on the surface. The increase of the ratio of Co/Fe on the surface has an influence on the malic acid conversion and on the pyruvic acid yield, while the yield of malonic acid is influenced by the percentage of iron on the surface (determined from XPS). Oxaloacetic acid yield reaches a maximumat one hour of reaction, being higher when ethanol is used as a solvent, after which it suddenly decreases. The hydrogenation of malic acid occurs by consecutive reactions with the production of 3-hydroxy-butyrolactone, 1,2,4-butanetriol and 1,4-butanediol. Malic acid conversion increases with cobalt loading increasing up to Co/Fe ratio of 0.1, after which it has a slight decrease, while the yield in 1,4-butanediol is directly proportional to the cobalt content.

Keywords: malic acid, oxidative dehydrogenation, hydrogenation, oxaloacetic acid

Procedia PDF Downloads 159

Authors: K. Mohon Singh

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Cambro-Ordovician (512.5 ± 8.7 Ma) felsic magmatism in the Kyrdem region of Meghalaya plateau, herewith referred to as Kyrdem granitoids (KG), intrudes the low-grade Shillong Group of metasediments and Precambrian Basement Gneissic complex forming an oval-shaped plutonic body with longer axis almost trending N-S. Thermal aureole is poorly developed or covered under the alluvium. KG exhibit very coarse grained porphyritic texture with abundant K-feldspar megacrysts (up to 9cm long) and subordinate amount of amphibole, biotite, plagioclase, and quartz. The size of K-feldspar megacrysts increases from margin (Dwarksuid) to the interior (Kyrdem) of the KG pluton. Late felsic pulses as fine grained granite, leucocratic (aplite), and pegmatite veins intrude the KG at several places. Grey and pink varieties of KG can be recognized, but pink colour of KG is the result of post-magmatic fluids, which have not affected the magnetic properties of KG. Modal composition of KG corresponds to quartz monzonite, monzogranite, and granodiorite. KG has been geochemically characterized as metaluminous (I-type) to peraluminous (S-type) granitoids. The KG is characterized by development of variable attitude of primary foliations mostly marked along the margin of the pluton and is located at the proximity of Tyrsad-Barapani lineament. The KG contains country rock xenoliths (amphibolite, gneiss, schist, etc.) which are mostly confined to the margin of the pluton, and microgranular enclaves (ME) are hosted in the porphyritic variety of KG. Microgranular Enclaves (ME) in Kyrdem Granitoids are fine- to medium grained, mesocratic to melanocratic, phenocryst bearing or phenocryst-free, rounded to ellipsoidal showing typical magmatic textures. Mafic-felsic phenocrysts in ME are partially corroded and dissolved because of their involvement in magma-mixing event, and thus represent xenocrysts. Sharp to diffused contacts of ME with host Kyrdem Granitoids, fine grained nature and presence of acicular apatite in ME suggest comingling and undercooling of coeval, semi-solidified ME magma within partly crystalline felsic host magma. Geochemical features recognize the nature of ME (molar A/CNK=0.76-1.42) and KG (molar A/CNK =0.41-1.75) similar to hybrid-type formed by mixing of mantle-derived mafic and crustal-derived felsic magmas. Major and trace including rare earth elements variations of ME suggest the involvement of combined processes such as magma mixing, mingling and crystallization differentiation in the evolution of ME but KG variations appear primarily controlled by fractionation of plagioclase, hornblende biotite, and accessory phases. Most ME are partially to nearly re-equilibrate chemically with felsic host KG during magma mixing and mingling processes.

Keywords: geochemistry, Kyrdem Granitoids, microgranular enclaves, Northeast India

Procedia PDF Downloads 102

Authors: Sh. Sousani, Z. Shadrokh, M. Hofbauerová, J. Kollár, M. Jergel, P. Nádaždy, M. Omastová, E. Majková

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Perovskite quantum dots (PQDs) have the potential to increase the performance of the perovskite solar cell (PSCs). The integration of PQDs into PSCs can extend the absorption range and enhance photon harvesting and device efficiency. In addition, PQDs can stabilize the device structure by passivating surface defects and traps in the perovskite layer and enhance its stability. The integration of PQDs into PSCs is strongly affected by the type of ligands on the surface of PQDs. The ligands affect the charge transport properties of PQDs, as well as the formation of well-defined interfaces and stability of PSCs. In this work, the CsPbBr₃ QDs were synthesized by the conventional hot-injection method using cesium oleate, PbBr₂ and two different ligands, namely oleic acid (OA) oleylamine (OAm) and didodecyldimethylammonium bromide (DDAB). The STEM confirmed regular shape and relatively monodisperse cubic structure with an average size of about 10-14 nm of the prepared CsPbBr₃ QDs. Further, the photoluminescent (PL) properties of the PQDs/perovskite bilayer with the ligand OA, OAm and DDAB were studied. For this purpose, ITO/PQDs as well as ITO/PQDs/MAPI perovskite structures were prepared by spin coating and the effect of the ligand and oxygen plasma treatment was analyzed. The plasma treatment of the PQDs layer could be beneficial for the deposition of the MAPI perovskite layer and the formation of a well-defined PQDs/MAPI interface. The absorption edge in UV-Vis absorption spectra for OA, OAm CsPbBr₃ QDs is placed around 513 nm (the band gap 2.38 eV); for DDAB CsPbBr₃ QDs, it is located at 490 nm (the band gap 2.33 eV). The photoluminescence (PL) spectra of CsPbBr₃ QDs show two peaks located around 514 nm (503 nm) and 718 nm (708 nm) for OA, OAm (DDAB). The peak around 500 nm corresponds to the PL of PQDs, and the peak close to 710 nm belongs to the surface states of PQDs for both types of ligands. These surface states are strongly affected by the O₃ plasma treatment. For PQDs with DDAB ligand, the O₃ exposure (5, 10, 15 s) results in the blue shift of the PQDs peak and a non-monotonous change of the amplitude of the surface states' peak. For OA, OAm ligand, the O₃ exposition did not cause any shift of the PQDs peak, and the intensity of the PL peak related to the surface states is lower by one order of magnitude in comparison with DDAB, being affected by O₃ plasma treatment. The PL results indicate the possibility of tuning the position of the PL maximum by the ligand of the PQDs. Similar behavior of the PQDs layer was observed for the ITO/QDs/MAPI samples, where an additional strong PL peak at 770 nm coming from the perovskite layer was observed; for the sample with PQDs with DDAB ligands, a small blue shift of the perovskite PL maximum was observed independently of the plasma treatment. These results suggest the possibility of affecting the PL maximum position and the surface states of the PQDs by the combination of a suitable ligand and the O₃ plasma treatment.

Keywords: perovskite quantum dots, photoluminescence, O₃ plasma., Perovskite Solar Cells

Procedia PDF Downloads 43

Authors: Sh. Sousani, Z. Shadrokh, M. Hofbauerová, J. Kollár, M. Jergel, P. Nádaždy, M. Omastová, E. Majková

Abstract:

Perovskite quantum dots (PQDs) have the potential to increase the performance of the perovskite solar cells (PSCs). The integration of PQDs into PSCs can extend the absorption range and enhance photon harvesting and device efficiency. In addition, PQDs can stabilize the device structure by passivating surface defects and traps in the perovskite layer and enhance its stability. The integration of PQDs into PSCs is strongly affected by the type of ligands on the surface of PQDs. The ligands affect the charge transport properties of PQDs, as well as the formation of well-defined interfaces and stability of PSCs. In this work, the CsPbBr₃ QDs were synthesized by the conventional hot-injection method using cesium oleate, PbBr₂, and two different ligands, namely oleic acid (OA)@oleylamine (OAm) and didodecyldimethylammonium bromide (DDAB). The STEM confirmed regular shape and relatively monodisperse cubic structure with an average size of about 10-14 nm of the prepared CsPbBr₃ QDs. Further, the photoluminescent (PL) properties of the PQDs/perovskite bilayer with the ligand OA@OAm and DDAB were studied. For this purpose, ITO/PQDs, as well as ITO/PQDs/MAPI perovskite structures, were prepared by spin coating, and the effect of the ligand and oxygen plasma treatment was analysed. The plasma treatment of the PQDs layer could be beneficial for the deposition of the MAPI perovskite layer and the formation of a well-defined PQDs/MAPI interface. The absorption edge in UV-Vis absorption spectra for OA@OAm CsPbBr₃ QDs is placed around 513 nm (the band gap 2.38 eV); for DDAB CsPbBr₃ QDs, it is located at 490 nm (the band gap 2.33 eV). The photoluminescence (PL) spectra of CsPbBr₃ QDs show two peaks located around 514 nm (503 nm) and 718 nm (708 nm) for OA@OAm (DDAB). The peak around 500 nm corresponds to the PL of PQDs, and the peak close to 710 nm belongs to the surface states of PQDs for both types of ligands. These surface states are strongly affected by the O₃ plasma treatment. For PQDs with DDAB ligand, the O₃ exposure (5, 10, 15 s) results in the blue shift of the PQDs peak and a non-monotonous change of the amplitude of the surface states' peak. For OA@OAm ligand, the O₃ exposition did not cause any shift of the PQDs peak, and the intensity of the PL peak related to the surface states is lower by one order of magnitude in comparison with DDAB, being affected by O₃ plasma treatment. The PL results indicate the possibility of tuning the position of the PL maximum by the ligand of the PQDs. Similar behaviour of the PQDs layer was observed for the ITO/QDs/MAPI samples, where an additional strong PL peak at 770 nm coming from the perovskite layer was observed; for the sample with PQDs with DDAB ligands, a small blue shift of the perovskite PL maximum was observed independently of the plasma treatment. These results suggest the possibility of affecting the PL maximum position and the surface states of the PQDs by the combination of a suitable ligand and the O₃ plasma treatment.

Keywords: perovskite quantum dots, photoluminescence, O₃ plasma., perovskite solar cells

Procedia PDF Downloads 46

Authors: Karolina Ordon, Sandrine Coste, Malgorzata Makowska-Janusik, Abdelhadi Kassiba

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Photocatalytic processes play key role in the production of a new source of energy (as hydrogen), design of self-cleaning surfaces or for the environment preservation. The most challenging task deals with the purification of water distinguished by high efficiency. In the mentioned process, organic pollutants in solutions are decomposed to the simple, non-toxic compounds as H2O and CO2. The most known photocatalytic materials are ZnO, CdS and TiO2 semiconductors with a particular involvement of TiO2 as an efficient photocatalysts even with a high band gap equal to 3.2 eV which exploit only UV radiation from solar emitted spectrum. However, promising material with visible light induced photoactivity was searched through the monoclinic polytype of BiVO4 which has energy gap about 2.4 eV. As required in heterogeneous photocatalysis, the high contact surface is required. Also, BiVO4 as photocatalyst can be optimized by increasing its surface area by achieving the mesoporous structure synthesize. The main goal of the present work consists in the synthesis and characterization of BiVO4 mesoporous thin film. The synthesis method based on sol-gel was carried out using a standard surfactants such as P123 and F127. The thin film was deposited by spin and dip coating method. Then, the structural analysis of the obtained material was performed thanks to X-ray diffraction (XRD) and Raman spectroscopy. The surface of resulting structure was investigated using a scanning electron microscopy (SEM). The computer simulations based on modeling the optical and electronic properties of bulk BiVO4 by using DFT (density functional theory) methodology were carried out. The semiempirical parameterized method PM6 was used to compute the physical properties of BiVO4 nanostructures. The Raman and IR absorption spectra were also measured for synthesized mesoporous material, and the results were compared with the theoretical predictions. The simulations of nanostructured BiVO4 have pointed out the occurrence of quantum confinement for nanosized clusters leading to widening of the band gap. This result overcame the relevance of nanosized objects to harvest wide part of the solar spectrum. Also, a balance was searched experimentally through the mesoporous nature of the films devoted to enhancing the contact surface as required for heterogeneous catalysis without to lower the nanocrystallite size under some critical sizes inducing an increased band gap. The present contribution will discuss the relevant features of the mesoporous films with respect to their photocatalytic responses.

Keywords: bismuth vanadate, photocatalysis, thin film, quantum-chemical calculations

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Authors: Su Yin Chiam, Zhipeng Ding, Guang Yang, Danny Jian Hang Tng, Peiyi Song, Geok Ing Ng, Ken-Tye Yong, Qing Xin Zhang

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Brain-machine interfaces (BMI) is a ground rich of exploration opportunities where manipulation of neural activity are used for interconnect with myriad form of external devices. These research and intensive development were evolved into various areas from medical field, gaming and entertainment industry till safety and security field. The technology were extended for neurological disorders therapy such as obsessive compulsive disorder and Parkinson’s disease by introducing current pulses to specific region of the brain. Nonetheless, the work to develop a real-time observing, recording and altering of neural signal brain-machine interfaces system will require a significant amount of effort to overcome the obstacles in improving this system without delay in response. To date, feature size of interface devices and the density of the electrode population remain as a limitation in achieving seamless performance on BMI. Currently, the size of the BMI devices is ranging from 10 to 100 microns in terms of electrodes’ diameters. Henceforth, to accommodate the single cell level precise monitoring, smaller and denser Nano-scaled nanowire electrode arrays are vital in fabrication. In this paper, we would like to showcase the fabrication of high aspect ratio of vertical silicon nanowire electrodes arrays using microelectromechanical system (MEMS) method. Nanofabrication of the nanowire electrodes involves in deep reactive ion etching, thermal oxide thinning, electron-beam lithography patterning, sputtering of metal targets and bottom anti-reflection coating (BARC) etch. Metallization on the nanowire electrode tip is a prominent process to optimize the nanowire electrical conductivity and this step remains a challenge during fabrication. Metal electrodes were lithographically defined and yet these metal contacts outline a size scale that is larger than nanometer-scale building blocks hence further limiting potential advantages. Therefore, we present an integrated contact solution that overcomes this size constraint through self-aligned Nickel silicidation process on the tip of vertical silicon nanowire electrodes. A 4 x 4 array of vertical silicon nanowires electrodes with the diameter of 290nm and height of 3µm has been successfully fabricated.

Keywords: brain-machine interfaces, microelectromechanical systems (MEMS), nanowire, nickel silicide

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Authors: Marta Paszkiewicz, Justyna Łuczak, Martyna Marchelek, Adriana Zaleska-Medynska

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In recent years, photocatalytical processes have been intensively investigated for destruction of pollutants, hydrogen evolution, disinfection of water, air and surfaces, for the construction of self-cleaning materials (tiles, glass, fibres, etc.). Titanium dioxide (TiO2) is the most popular material used in heterogeneous photocatalysis due to its excellent properties, such as high stability, chemical inertness, non-toxicity and low cost. It is well known that morphology and microstructure of TiO2 significantly influence the photocatalytic activity. This characteristics as well as other physical and structural properties of photocatalysts, i.e., specific surface area or density of crystalline defects, could be controlled by preparation route. In this regard, TiO2 particles can be obtained by sol-gel, hydrothermal, sonochemical methods, chemical vapour deposition and alternatively, by ionothermal synthesis using ionic liquids (ILs). In the TiO2 particles synthesis ILs may play a role of a solvent, soft template, reagent, agent promoting reduction of the precursor or particles stabilizer during synthesis of inorganic materials. In this work, the effect of the ILs anion type on morphology and photoactivity of TiO2 is presented. The preparation of TiO2 microparticles with spherical structure was successfully achieved by solvothermal method, using tetra-tert-butyl orthotitatane (TBOT) as the precursor. The reaction process was assisted by an ionic liquids 1-butyl-3-methylimidazolium bromide [BMIM][Br], 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF4] and 1-butyl-3-methylimidazolium haxafluorophosphate [BMIM][PF6]. Various molar ratios of all ILs to TBOT (IL:TBOT) were chosen. For comparison, reference TiO2 was prepared using the same method without IL addition. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Brenauer-Emmett-Teller surface area (BET), NCHS analysis, and FTIR spectroscopy were used to characterize the surface properties of the samples. The photocatalytic activity was investigated by means of phenol photodegradation in the aqueous phase as a model pollutant, as well as formation of hydroxyl radicals based on detection of fluorescent product of coumarine hydroxylation. The analysis results showed that the TiO2 microspheres had spherical structure with the diameters ranging from 1 to 6 µm. The TEM micrographs gave a bright observation of the samples in which the particles were comprised of inter-aggregated crystals. It could be also observed that the IL-assisted TiO2 microspheres are not hollow, which provides additional information about possible formation mechanism. Application of the ILs results in rise of the photocatalytic activity as well as BET surface area of TiO2 as compared to pure TiO2. The results of the formation of 7-hydroxycoumarin indicated that the increased amount of ·OH produced at the surface of excited TiO2 for samples TiO2_ILs well correlated with more efficient degradation of phenol. NCHS analysis showed that ionic liquids remained on the TiO2 surface confirming structure directing role of that compounds.

Keywords: heterogeneous photocatalysis, IL-assisted synthesis, ionic liquids, TiO2

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Authors: Giorgi Chichinadze, David Shengelia, Tamara Tsutsunava, Nikoloz Maisuradze, Giorgi Beridze

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The Jalovchat gabbro intrusive is exposed on the northern and southern slopes of Main Range zone of the Greater Caucasus, on an area about 25km2. It is intruded in Precambrian crystalline schists and amphibolites intensively metamorphose them along the contact zone. The intrusive is represented by hornblende-bearing gabbro, gabbro-norites and norites including thin vein bodies of gabbro-pegmatites, anorthosites and micro-gabbros. Especially should be noted the veins of gabbro-pegmatites with the gigantic (up to 0.5m) hornblende crystals. From this point of view, the Jalovchat gabbroid intrusive is particularly interesting and by its unusual composition has no analog in the Caucasus overall. The comprehensive petrologic and geochemical study of the intrusive was carried out by the authors. The results of investigations are following. Amphiboles correspond to magnesiohastingsite and magnesiohornblende. In hastingsite and hornblende as a result of isovalent isomorphism of Fe2+ by Mg, content of the latter has been increased. By AMF and Na20+K diagrams the intrusive rocks correspond to tholeiitic basalts or to basalts close to it by composition. According to ACM-AMF double diagram the samples distributed in the fields of MORB and alkali cumulates. In TiO2/FeO+Fe2O3, Zr/Y-Zr and Ti-Cr/Ni diagrams and Ti-Cr-Y triangular diagram samples are arranged in the fields of island-arc and mid-oceanic basalts or along the trends reflecting mid-oceanic ridges or island arcs. K2O/TiO2 diagram shows that these rocks belong to normal and enriched MORB type. According to Th/Nb/Y ratio, the Jalovchat intrusive composition corresponds to depleted mantle, but by Sm/Y-Ce/Sm - to the MORB area. Th/Y and Nb/Y ratios coincide with the MORB composition, Th/Yb-Ta/Yb and La/Nb-Ti ratios correspond to N MORB, and Rb/Y and N/Y - to the lower crust formations. Exceptional are Ce/Pb-Ce and Nb/Th-Nb diagrams, showing the area of primitive mantle. Spidergrams are characterized by almost horizontal trend, weakly expressed Eu minimums and by a slight depletion of light REE. Similar are characteristic of typical tholeiit basalts. In comparison to MORB spidergrams, they are characterized by depletion of light REE. Their correlation to the spidergrams of Jalovchat intrusive proves that they are more depleted. The above cited points to the gradual depletion of mantle with the light REE in geological time. The RE and REE diagrams reveal unexpected regularity. In particular, petro-geochemical characteristics of Jalovchat gabbroid intrusive predominantly correspond to MORB, that usually is an anomalous phenomenon, since in ‘ophiolitic’ section magmatic formations represented mainly by gigantic prismatic hornblende-bearing gabbro and gabbro-pegmatite are not indicated. On the basis of petro-mineralogical and petro-geochemical data analysis, the authors consider that the Jalovchat intrusive belongs to the subduction geodynamic type. In the depleted mantle rich in water the MORB rock system has subducted, where the favorable conditions for crystallization of hornblende and especially for its gigantic crystals occurred. It is considered that the Jalovchat intrusive was formed in deep horizons of the Earth’s crust as a result of crystallization of water-bearing Bajocian basalt magma.

Keywords: The Greater Caucasus, gabbro-pegmatite, hornblende-bearing gabbro, petrogenesis

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Authors: Aura Maria Lopera Echavarria, Angela Maria Lema Perez, Daniela Medrano David, Pedronel Araque Marin, Marta Elena Londoño Lopez

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Bone regeneration is the process by which the formation of new bone is stimulated. Bone fractures can originate at any time due to trauma, infections, tumors, congenital malformations or skeletal diseases. Currently there are different strategies to treat bone defects that in some cases, regeneration does not occur on its own. That is why they are treated with bone substitutes, which provide a necessary environment for the cells to synthesize new bone. The Demineralized Bone Matrix (DBM) is widely used as a bone implant due to its good properties, such as osteoinduction and bioactivity. However, the use of DBM is limited, because its presentation is powder, which is difficult to implant with precision and is susceptible to migrating to other sites through blood flow. That is why the DBM is commonly incorporated into a variety of vehicles or carriers. The objective of this project is to evaluate the bioactive and confinement properties of a bone substitute based on demineralized bone matrix (DBM). Also, structural and morphological properties were evaluated. Bone substitute was obtained from EIA Biomaterials Laboratory of EIA University and the DBM was facilitated by Tissue Bank Foundation. Morphological and structural properties were evaluated by scanning electron microscopy (SEM), X-ray diffraction (DRX) and Fourier transform infrared spectroscopy with total attenuated reflection (FTIR-ATR). Water absorption capacity and degradation were also evaluated during three months. The cytotoxicity was evaluated by the MTT test. The bioactivity of the bone substitute was evaluated through immersion of the samples in simulated body fluid during four weeks. Confinement tests were performed on tibial fragments of a human donor with bone defects of determined size, to ensure that the substitute remains in the defect despite the continuous flow of fluid. According of the knowledge of the authors, the methodology for evaluating samples in a confined environment has not been evaluated before in real human bones. The morphology of the samples showed irregular surface and presented some porosity. DRX confirmed a semi-crystalline structure. The FTIR-ATR determined the organic and inorganic phase of the sample. The degradation and absorption measurements stablished a loss of 3% and 150% in one month respectively. The MTT showed that the system is not cytotoxic. Apatite clusters formed from the first week were visualized by SEM and confirmed by EDS. These calcium phosphates are necessary to stimulate bone regeneration and thanks to the porosity of the developed material, osteinduction and osteoconduction are possible. The results of the in vitro evaluation of the confinement of the material showed that the migration of the bone filling to other sites is negligible, although the samples were subjected to the passage of simulated body fluid. The bone substitute, putty type, showed stability, is bioactive, non-cytotoxic and has handling properties for specialists at the time of implantation. The obtained system allows to maintain the osteoinductive properties of DBM and it can fill completely fractures in any way; however, it does not provide a structural support, that is, it should only be used to treat fractures without requiring a mechanical load.

Keywords: bone regeneration, cytotoxicity, demineralized bone matrix, hydrogel

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Authors: Muccifora S., Rinallo C., Bellani L.

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Calcium (Ca²+) is an element essential to the plant being involved in plant growth and development. At high concentrations, it is toxic and can influence every stage, process and cellular activity of plant life. Given its toxicity, cells implement mechanisms to compartmentalize calcium in a vacuole, endoplasmic reticulum, mitochondria, plastids and cell wall. One of the most effective mechanisms to reduce the excess of calcium, thus avoiding cellular damage, is its complexation with oxalic acid to form calcium oxalate crystals that are no longer osmotically or physiologically active. However, the sequestered calcium can be mobilized when the plant needs it. Calcium crystals can be accumulated in the vacuole of specialized sink-cells called idioblasts, with different crystalline forms (druse, raphyde and styloid) of diverse physiological meanings. Actinidia deliciosa cv. Hayward presents raphydes and styloid localized in idioblasts in cells of photosynthetic and non-photosynthetic tissues. The purpose of this work was to understand if there is a relationship between the age of Actinidia leaves and the presence, distribution, dimension and shape of oxalate crystals by means of light, fluorescent, polarized and transmission electron microscopy. Three vines from female plants were chosen at the beginning of the season and used throughout the study. The leaves with petioles were collected at various stages of development from the bottom to the shoot of the plants monthly from April to July. The samples were taken in corresponding areas of the central and lateral parts of the leaves and of the basal portion of the petiole. The results showed that in the leaves, the number of raphyde idioblasts decreased with the progress of the growing season, while the styloid idioblasts increased progressively, becoming very numerous in the upper nodes of July. In June and in July samples, in the vacuoles of the highest nodes, a portion regular in shape strongly stained with rubeanic acid was present. Moreover, the chlortetracycline (CTC) staining for localization of free calcium marked the wall of the idioblasts and the wall of the cells near vascular bundles. In April petiole samples, moving towards the youngest nodes, the raphydes idioblast decreased in number and in the length of the single raphydes. Besides, crystals stained with rubeanic acid appeared in the vacuoles of some cells. In June samples, numerous raphyde idioblasts oriented parallel to vascular bundles were evident. Under the electron microscope, numerous idioblasts presented not homogeneous electrondense aggregates of material, in which a few crystals (styloids) in the form of regular holes were scattered. In July samples, an increase in the number of styloid idioblasts in the youngest nodes and little masses stained with CTC near styloids were observed. Peculiar cells stained with rubeanic acid were detected and hypothesized to be involved in the formation of the idioblasts. In conclusion, in Actinidia leaves and petioles, it seems to confirm the hypothesis that the formation of styloid idioblasts can be correlated to increasing calcium levels in growing tissues.

Keywords: calcium oxalate crystals, actinidia deliciosa, light and electron microscopy, idioblasts

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Authors: Małgorzata Golonka, Jadwiga Laska

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Self-healing polymers are one of the most investigated groups of smart materials. As materials engineering has recently focused on the design, production and research of modern materials and future technologies, researchers are looking for innovations in structural, construction and coating materials. Based on available scientific articles, it can be concluded that most of the research focuses on the self-healing of cement, concrete, asphalt and anticorrosion resin coatings. In our study, a method of obtaining and testing the properties of several types of microcapsules for use in self-healing polymer materials was developed. A method to obtain microcapsules exhibiting various mechanical properties, especially compressive strength was developed. The effect was achieved by using various polymer materials to build the shell: urea-formaldehyde resin (UFR), melamine-formaldehyde resin (MFR), melamine-urea-formaldehyde resin (MUFR). Dicyclopentadiene (DCPD) was used as the core material due to the possibility of its polymerization according to the ring-opening olefin metathesis (ROMP) mechanism in the presence of a solid Grubbs catalyst showing relatively high chemical and thermal stability. The ROMP of dicyclopentadiene leads to a polymer with high impact strength, high thermal resistance, good adhesion to other materials and good chemical and environmental resistance, so it is potentially a very promising candidate for the self-healing of materials. The capsules were obtained by condensation polymerization of formaldehyde with urea, melamine or copolymerization with urea and melamine in situ in water dispersion, with different molar ratios of formaldehyde, urea and melamine. The fineness of the organic phase dispersed in water, and consequently the size of the microcapsules, was regulated by the stirring speed. In all cases, to establish such synthesis conditions as to obtain capsules with appropriate mechanical strength. The microcapsules were characterized by determining the diameters and their distribution and measuring the shell thickness using digital optical microscopy and scanning electron microscopy, as well as confirming the presence of the active substance in the core by FTIR and SEM. Compression tests were performed to determine mechanical strength of the microcapsules. The highest repeatability of microcapsule properties was obtained for UFR resin, while the MFR resin had the best mechanical properties. The encapsulation efficiency of MFR was much lower compared to UFR, though. Therefore, capsules with a MUFR shell may be the optimal solution. The chemical reaction between the active substance present in the capsule core and the catalyst placed outside the capsules was confirmed by FTIR spectroscopy. The obtained autonomous repair systems (microcapsules + catalyst) were introduced into polyethylene in the extrusion process and tested for the self-repair of the material.

Keywords: autonomic self-healing system, dicyclopentadiene, melamine-urea-formaldehyde resin, microcapsules, thermoplastic materials

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Authors: Olagunju John Olusesan-Remi

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The study area Ijero-Ekiti falls within the Ilesha-Ekiti Schist belt, originating from the long year of the Pan-Africa orogenic events and various cataclysmic tectonic activities in history. Ijero-Ekiti is situated within latitude 7 degree 45N and 7 Degree 55N. Ijero Ekiti is bordered between the Dahomean Basin and the southern Bida/Benue basin on the Geological map of Nigeria. This research work centers on majorly on investigating the chemical composition and as well as the mineralogical distribution of the various mineral-bearing rocks that composed the study area. This work is essentially carried out with a view to assessing and at the same time ascertaining the economic potentials and or the industrial significance of the area to Ekiti-south western region and the Nigeria nation as a whole. The mineralogical distribution pattern is of particular interest to us in this study. In this regard essential focus is put on the mostly the economic gemstones distributions within the various mineral bearing rocks in the zone, some of which includes the tourmaline formation, cassiterite deposit, tin-ore, tantalum columbite, smoky quartz, amethyst, polychrome and emerald variety beryl among others as they occurred within the older granite of the Precambrian rocks. To this end, samples of the major rock types were taken from various locations within the study area for detail scientific analysis as follows: The Igemo pegmatite of Ijero west, the epidiorite of Idaho, the biotitic hornblende gneiss of Ikoro-Ijero north and the beryl crystalline rock types to mention a few. The slides of the each rock from the aforementioned zones were later prepared and viewed under a cross Nichol petro graphic microscope with a particular focus on the light reflection ability of the constituent minerals in each rock samples. The results from the physical analysis viewed from the colour had it that the pegmatite samples ranges from pure milky white to fairly pinkish coloration. Other physical properties investigated include the streak, luster, form, specific gravity, cleavage/fracture pattern etc. The optical examination carried out centers on the refractive indices and pleochroism of the minerals present while the chemical analysis reveals from the tourmaline samples a differing correlation coefficient of the various oxides in each samples collected through which the mineral presence was established. In conclusion, it was inferred that the various minerals outlined above were in reasonable quantity within the Ijero area. With the above discoveries, therefore, we strongly recommend a detailed scientific investigation to be carried out such that will lead to a comprehensive mining of the area. Above all, it is our conclusion that a comprehensive mineralogical exploitation of this area will not only boost the socio-economic potential of the area but at the same time will go a long way contributing immensely to the socio-economic growth and development of the Nation-Nigeria at large.

Keywords: Ijero Ekiti, Southwestern Nigeria, economic minerals, pegmatite of the pan African origin, cataclastic tectonic activities, Ilesha Schistbelt, precambrian formations

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Authors: Simon Grossemy, Peggy P. Y. Chan, Pauline M. Doran

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Nerve tissue engineering is the main field of research aimed at finding an alternative to autografts as a treatment for nerve injuries. Scaffolds are used as a support to enhance nerve regeneration. In order to successfully design novel scaffolds and in vitro cell culture systems, a deep understanding of the factors affecting nerve regeneration processes is needed. Physical and biological parameters associated with the culture environment have been identified as potentially influential in nerve cell differentiation, including electrical stimulation, exposure to extracellular-matrix (ECM) proteins, dynamic medium conditions and co-culture with glial cells. The mechanisms involved in driving the cell to differentiation in the presence of these factors are poorly understood; the complexity of each of them raises the possibility that they may strongly influence each other. Some questions that arise in investigating nerve regeneration include: What are the best protein coatings to promote neural cell attachment? Is the scaffold design suitable for providing all the required factors combined? What is the influence of dynamic stimulation on cell viability and differentiation? In order to study these effects, scaffolds adaptable to bioreactor culture conditions were designed to allow electrical stimulation of cells exposed to ECM proteins, all within a dynamic medium environment. Gold coatings were used to make the surface of viscose rayon microfiber scaffolds (VRMS) conductive, and poly-L-lysine (PLL) and laminin (LN) surface coatings were used to mimic the ECM environment and allow the attachment of rat PC12 neural cells. The robustness of the coatings was analyzed by surface resistivity measurements, scanning electron microscope (SEM) observation and immunocytochemistry. Cell attachment to protein coatings of PLL, LN and PLL+LN was studied using DNA quantification with Hoechst. The double coating of PLL+LN was selected based on high levels of PC12 cell attachment and the reported advantages of laminin for neural differentiation. The underlying gold coatings were shown to be biocompatible using cell proliferation and live/dead staining assays. Coatings exhibiting stable properties over time under dynamic fluid conditions were developed; indeed, cell attachment and the conductive power of the scaffolds were maintained over 2 weeks of bioreactor operation. These scaffolds are promising research tools for understanding complex neural cell behavior. They have been used to investigate major factors in the physical culture environment that affect nerve cell viability and differentiation, including electrical stimulation, bioreactor hydrodynamic conditions, and combinations of these parameters. The cell and tissue differentiation response was evaluated using DNA quantification, immunocytochemistry, RT-qPCR and functional analyses.

Keywords: bioreactor, electrical stimulation, nerve differentiation, PC12 cells, scaffold

Procedia PDF Downloads 219

Authors: M. Vezir Kahraman, Emre Basturk

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Energy storage technology offers new ways to meet the demand to obtain efficient and reliable energy storage materials. Thermal energy storage systems provide the potential to acquire energy savings, which in return decrease the environmental impact related to energy usage. For this purpose, phase change materials (PCMs) that work as 'latent heat storage units' which can store or release large amounts of energy are preferred. Phase change materials (PCMs) are being utilized to absorb, collect and discharge thermal energy during the cycle of melting and freezing, converting from one phase to another. Phase Change Materials (PCMs) can generally be arranged into three classes: organic materials, salt hydrates and eutectics. Many kinds of organic and inorganic PCMs and their blends have been examined as latent heat storage materials. PCMs have found different application areas such as solar energy storage and transfer, HVAC (Heating, Ventilating and Air Conditioning) systems, thermal comfort in vehicles, passive cooling, temperature controlled distributions, industrial waste heat recovery, under floor heating systems and modified fabrics in textiles. Ultraviolet (UV)-curing technology has many advantages, which made it applicable in many different fields. Low energy consumption, high speed, room-temperature operation, low processing costs, high chemical stability, and being environmental friendly are some of its main benefits. UV-curing technique has many applications. One of the many advantages of UV-cured PCMs is that they prevent the interior PCMs from leaking. Shape-stabilized PCM is prepared by blending the PCM with a supporting material, usually polymers. In our study, this problem is minimized by coating the fatty alcohols with a photo-cross-linked thiol-ene based polymeric system. Leakage is minimized because photo-cross-linked polymer acts a matrix. The aim of this study is to introduce a novel thiol-ene based shape-stabilized PCM. Photo-crosslinked thiol-ene based polymers containing fatty alcohols were prepared and characterized for the purpose of phase change materials (PCMs). Different types of fatty alcohols were used in order to investigate their properties as shape-stable PCMs. The structure of the PCMs was confirmed by ATR-FTIR techniques. The phase transition behaviors, thermal stability of the prepared photo-crosslinked PCMs were investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). This work was supported by Marmara University, Commission of Scientific Research Project.

Keywords: differential scanning calorimetry (DSC), Polymeric phase change material, thermal energy storage, UV-curing

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Authors: Tatiana S. Ogneva

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Aluminum and nickel-based intermetallic compounds have attracted the attention of scientific community as promising materials for heat-resistant and wear-resistant coatings in such manufacturing areas as microelectronics, aircraft and rocket building and chemical industries. Magnetron sputtering makes possible to coat materials without formation of liquid phase and improves the mechanical and functional properties of nickel aluminides due to the possibility of nanoscale structure formation. The purpose of the study is the investigation of structure and properties of intermetallic coatings produced by magnetron sputtering technique. The feature of this work is the using of composite targets for sputtering, which were consisted of two semicircular sectors of cp-Ni and cp-Al. Plates of alumina, silicon, titanium and steel alloys were used as substrates. To estimate sputtering conditions on structure of intermetallic coatings, a series of samples were produced and studied in detail using scanning and transition electron microcopy and X-Ray diffraction. Besides, nanohardness and scratching tests were carried out. The varying parameters were the distance from the substrate to the target, the duration and the power of the sputtering. The thickness of the obtained intermetallic coatings varied from 0.05 to 0.5 mm depending on the sputtering conditions. The X-ray diffraction data indicated that the formation of intermetallic compounds occurred after sputtering without additional heat treatment. Sputtering at a distance not closer than 120 mm led to the formation of NiAl phase. Increase in the power of magnetron from 300 to 900 W promoted the increase of heterogeneity of the phase composition and the appearance of intermetallic phases NiAl, Ni₂Al₃, NiAl₃, and Al under the aluminum side, and NiAl, Ni₃Al, and Ni under the nickel side of the target. A similar trend is observed with increasing the distance of sputtering from 100 to 60 mm. The change in the phase composition correlates with the changing of the atomic composition of the coatings. Scanning electron microscopy revealed that the coatings have a nanoscale grain structure. In this case, the substrate material and the distance from the substrate to the magnetron have a significant effect on the structure formation process. The size of nanograins differs from 10 to 83 nm and depends not only on the sputtering modes but also on material of a substrate. Nanostructure of the material influences the level of mechanical properties. The highest level of nanohardness of the coatings deposited during 30 minutes on metallic substrates at a distance of 100 mm reached 12 GPa. It was shown that nanohardness depends on the grain size of the intermetallic compound. Scratching tests of the coatings showed a high level of adhesion of the coating to substrate without any delamination and cracking. The results of the study showed that magnetron sputtering of composite targets consisting of nickel and aluminum semicircles makes it possible to form intermetallic coatings with good mechanical properties directly in the process of sputtering without additional heat treatment.

Keywords: intermetallic coatings, magnetron sputtering, mechanical properties, structure

Procedia PDF Downloads 104

Authors: Chee Wee Gan, Anthony Herr Cheun Ng, Yee Shan Wong, Subbu Venkatraman, Lynne Hsueh Yee Lim

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Otitis media with effusion (OME) is the leading cause of hearing loss in children worldwide. Surgery to insert grommet tube into the eardrum is usually indicated for OME unresponsive to antimicrobial therapy. It is the most common surgery for children. However, current commercially available grommet tubes are non-bioresorbable, not drug-treated, with unpredictable duration of retention on the eardrum to ventilate middle ear. Their functionality is impaired when clogged or chronically infected, requiring additional surgery to remove/reinsert grommet tubes. We envisaged that a novel fully bioresorbable grommet tube with sustained antibiotic release technology could address these drawbacks. In this study, drug-loaded bioresorbable poly(L-lactide-co-ε-caprolactone)(PLC) copolymer grommet tubes were fabricated by microinjection moulding technique. In vitro drug release and degradation model of PLC tubes were studied. Antibacterial property was evaluated by incubating PLC tubes with P. aeruginosa broth. Surface morphology was analyzed using scanning electron microscopy. A preliminary animal study was conducted using guinea pigs as an in vivo model to evaluate PLC tubes with and without drug, with commercial Mini Shah grommet tube as comparison. Our in vitro data showed sustained drug release over 3 months. All PLC tubes revealed exponential degradation profiles over time. Modeling predicted loss of tube functionality in water to be approximately 14 weeks and 17 weeks for PLC with and without drug, respectively. Generally, PLC tubes had less bacteria adherence, which were attributed to the much smoother tube surfaces compared to Mini Shah. Antibiotic from PLC tube further made bacteria adherence on surface negligible. They showed neither inflammation nor otorrhea after 18 weeks post-insertion in the eardrums of guinea pigs, but had demonstrated severe degree of bioresorption. Histology confirmed the new PLC tubes were biocompatible. Analyses on the PLC tubes in the eardrums showed bioresorption profiles close to our in vitro degradation models. The bioresorbable antibiotic-loaded grommet tubes showed good predictability in functionality. The smooth surface and sustained release technology reduced the risk of tube infection. Tube functional duration of 18 weeks allowed sufficient ventilation period to treat OME. Our ongoing studies include modifying the surface properties with protein coating, optimizing the drug dosage in the tubes to enhance their performances, evaluating their functional outcome on hearing after full resoption of grommet tube and healing of eardrums, and developing animal model with OME to further validate our in vitro models.

Keywords: bioresorbable polymer, drug release, grommet tube, guinea pigs, otitis media with effusion

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Authors: Esther Van Andel, Stefanie C. Lange, Maarten M. J. Smulders, Han Zuilhof

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False outcomes of diagnostic tests are a major concern in medical health care. To improve the reliability of surface-based diagnostic tests, it is of crucial importance to diminish background signals that arise from the non-specific binding of biomolecules, a process called fouling. The aim is to create surfaces that repel all biomolecules except the molecule of interest. This can be achieved by incorporating antifouling protein repellent coatings in between the sensor surface and it’s recognition elements (e.g. antibodies, sugars, aptamers). Zwitterionic polymer brushes are considered excellent antifouling materials, however, to be able to bind the molecule of interest, the polymer brushes have to be functionalized and so far this was only achieved at the expense of either antifouling or binding capacity. To overcome this limitation, we combined both features into one single monomer: a zwitterionic sulfobetaine, ensuring antifouling capabilities, equipped with a clickable azide moiety which allows for further functionalization. By copolymerizing this monomer together with a standard sulfobetaine, the number of azides (and with that the number of recognition elements) can be tuned depending on the application. First, the clickable azido-monomer was synthesized and characterized, followed by copolymerizing this monomer to yield functionalizable antifouling brushes. The brushes were fully characterized using surface characterization techniques like XPS, contact angle measurements, G-ATR-FTIR and XRR. As a proof of principle, the brushes were subsequently functionalized with biotin via strain-promoted alkyne azide click reactions, which yielded a fully zwitterionic biotin-containing 3D-functionalized coating. The sensing capacity was evaluated by reflectometry using avidin and fibrinogen containing protein solutions. The surfaces showed excellent antifouling properties as illustrated by the complete absence of non-specific fibrinogen binding, while at the same time clear responses were seen for the specific binding of avidin. A great increase in signal-to-noise ratio was observed, even when the amount of functional groups was lowered to 1%, compared to traditional modification of sulfobetaine brushes that rely on a 2D-approach in which only the top-layer can be functionalized. This study was performed on stoichiometric silicon nitride surfaces for future microring resonator based assays, however, this methodology can be transferred to other biosensor platforms which are currently being investigated. The approach presented herein enables a highly efficient strategy for selective binding with retained antifouling properties for improved signal-to-noise ratios in binding assays. The number of recognition units can be adjusted to a specific need, e.g. depending on the size of the analyte to be bound, widening the scope of these functionalizable surface coatings.

Keywords: antifouling, signal-to-noise ratio, surface functionalization, zwitterionic polymer brushes

Procedia PDF Downloads 287

Authors: Anitha Kandasamy, Thirumurugan Ramaiah

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Interestingly, organic materials exhibit large optical nonlinearity with quick responses and having the flexibility of molecular tailoring using computational modelling and favourable synthetic methodologies. Pyridine based organic compounds and carboxylic acid contained aromatic compounds play a crucial role in crystal engineering of NCS complexes that displays admirable optical nonlinearity with fast response and favourable physicochemical properties such as low dielectric constant, wide optical transparency and large laser damage threshold value requires for optoelectronics device applications. Based on these facts, it was projected to form an acentric molecule of π-conjugated system interaction with appropriately replaced electron donor and acceptor groups for achieving higher SHG activity in which quinoline-2-carboyxlic acid is chosen as an electron acceptor and capable of acting as an acid as well as a base molecule, while 2-amino-4-methylpyridine is used as an electron donor and previously employed in numerous proton transfer complexes for synthesis of NLO materials for optoelectronic applications. 2-amino-4-mehtylpyridinium quinoline-2-carboxylate molecular complex (2AQ) is having π-donor-acceptor groups in which 2-amino-4-methylpyridine donates one of its electron to quinoline -2-carboxylic acid thereby forming a protonated 2-amino-4-methyl pyridinium moiety and mono ionized quinoline-2-carboxylate moiety which are connected via N-H…O intermolecular interactions with non-centrosymmetric crystal packing arrangement at microscopic scale is accountable to the enhancement of macroscopic second order NLO activity. The 2AQ crystal was successfully grown by a slow evaporation solution growth technique and its structure was determined in orthorhombic crystal system with acentric, P212121, space group. Hirshfeld surface analysis reveals that O…H intermolecular interactions primarily contributed with 31.0 % to the structural stabilization of 2AQ. The molecular structure of title compound has been confirmed by 1H and 13C NMR spectral studies. The vibrational modes of functional groups present in 2AQ have been assigned by using FTIR and FT-Raman spectroscopy. The grown 2AQ crystal exhibits high optical transparency with lower cut-off wavelength (275 nm) within the region of 275-1500 nm. The laser study confirmed that 2AQ exhibits high SHG efficiency of 12.6 times greater than that of KDP. TGA-DTA analysis revealed that 2AQ crystal had a thermal stability of 223 °C. The low dielectric constant and low dielectric loss at higher frequencies confirmed good crystalline nature with fewer defects of grown 2AQ crystal. The grown crystal exhibits soft material and positive photoconduction behaviour. Mulliken atomic distribution and FMOs analysis suggested that the strong intermolecular hydrogen bonding which lead to the enhancement of NLO activity. These properties suggest that 2AQ crystal is a suitable material for optoelectronic and laser frequency conversion applications.

Keywords: crystal growth, NLO activity, proton transfer complex, quantum chemical investigation

Procedia PDF Downloads 105

Authors: Keping Zuo, Jia Yin Chia, Gideon Praveen Kumar Vijayakumar, Foad Kabinejadian, Fangsen Cui, Pei Ho, Hwa Liang Leo

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Carotid artery is the major vessel supplying blood to the brain. Carotid artery stenosis is one of the three major causes of stroke and the stroke is the fourth leading cause of death and the first leading cause of disability in most developed countries. Although there is an increasing interest in carotid artery stenting for treatment of cervical carotid artery bifurcation therosclerotic disease, currently available bare metal stents cannot provide an adequate protection against the detachment of the plaque fragments over diseased carotid artery, which could result in the formation of micro-emboli and subsequent stroke. Our research group has recently developed a novel preferential covered-stent for carotid artery aims to prevent friable fragments of atherosclerotic plaques from flowing into the cerebral circulation, and yet retaining the ability to preserve the flow of the external carotid artery. The preliminary animal studies have demonstrated the potential of this novel covered-stent design for the treatment of carotid therosclerotic stenosis. The purpose of this study is to evaluate the biomechanical property of PU membrane of different concentration configurations in order to refine the stent coating technique and enhance the clinical performance of our novel carotid covered stent. Results from this study also provide necessary material property information crucial for accurate simulation analysis for our stents. Method: Medical grade Polyurethane (ChronoFlex AR) was used to prepare PU membrane specimens. Different PU membrane configurations were subjected to uniaxial test: 22%, 16%, and 11% PU solution were made by mixing the original solution with proper amount of the Dimethylacetamide (DMAC). The specimens were then immersed in physiological saline solution for 24 hours before test. All specimens were moistened with saline solution before mounting and subsequent uniaxial testing. The specimens were preconditioned by loading the PU membrane sample to a peak stress of 5.5 Mpa for 10 consecutive cycles at a rate of 50 mm/min. The specimens were then stretched to failure at the same loading rate. Result: The results showed that the stress-strain response curves of all PU membrane samples exhibited nonlinear characteristic. For the ultimate failure stress, 22% PU membrane was significantly higher than 16% (p<0.05). In general, our preliminary results showed that lower concentration PU membrane is stiffer than the higher concentration one. From the perspective of mechanical properties, 22% PU membrane is a better choice for the covered stent. Interestingly, the hyperelastic Ogden model is able to accurately capture the nonlinear, isotropic stress-strain behavior of PU membrane with R2 of 0.9977 ± 0.00172. This result will be useful for future biomechanical analysis of our stent designs and will play an important role for computational modeling of our covered stent fatigue study.

Keywords: carotid artery, covered stent, nonlinear, hyperelastic, stress, strain

Procedia PDF Downloads 286

Authors: Daniel Sava, Dragos Gudovan, Iulia Alexandra Gudovan, Ioana Ardelean, Maria Sonmez, Denisa Ficai, Laurentia Alexandrescu, Ecaterina Andronescu

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Graphene and graphene oxide have been intensively studied due to the very good properties, which are intrinsic to the material or come from the easy doping of those with other functional groups. Graphene and graphene oxide have known a broad band of useful applications, in electronic devices, drug delivery systems, medical devices, sensors and opto-electronics, coating materials, sorbents of different agents for environmental applications, etc. The board range of applications does not come only from the use of graphene or graphene oxide alone, or by its prior functionalization with different moieties, but also it is a building block and an important component in many composite devices, its addition coming with new functionalities on the final composite or strengthening the ones that are already existent on the parent product. An attempt to improve the mechanical properties of polyamide elastomers by compounding with graphene oxide in the parent polymer composition was attempted. The addition of the graphene oxide contributes to the properties of the final product, improving the hardness and aging resistance. Graphene oxide has a lower hardness and textile strength, and if the amount of graphene oxide in the final product is not correctly estimated, it can lead to mechanical properties which are comparable to the starting material or even worse, the graphene oxide agglomerates becoming a tearing point in the final material if the amount added is too high (in a value greater than 3% towards the parent material measured in mass percentages). Two different types of tests were done on the obtained materials, the hardness standard test and the tensile strength standard test, and they were made on the obtained materials before and after the aging process. For the aging process, an accelerated aging was used in order to simulate the effect of natural aging over a long period of time. The accelerated aging was made in extreme heat. For all materials, FT-IR spectra were recorded using FT-IR spectroscopy. From the FT-IR spectra only the bands corresponding to the polyamide were intense, while the characteristic bands for graphene oxide were very small in comparison due to the very small amounts introduced in the final composite along with the low absorptivity of the graphene backbone and limited number of functional groups. In conclusion, some compositions showed very promising results, both in tensile strength test and in hardness tests. The best ratio of graphene to elastomer was between 0.6 and 0.8%, this addition extending the life of the product. Acknowledgements: The present work was possible due to the EU-funding grant POSCCE-A2O2.2.1-2013-1, Project No. 638/12.03.2014, code SMIS-CSNR 48652. The financial contribution received from the national project ‘New nanostructured polymeric composites for centre pivot liners, centre plate and other components for the railway industry (RONERANANOSTRUCT)’, No: 18 PTE (PN-III-P2-2.1-PTE-2016-0146) is also acknowledged.

Keywords: graphene, graphene oxide, mechanical properties, dopping effect

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Authors: Evgeniya Orlova, Dmitriy Feoktistov, Geniy Kuznetsov

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Spreading of a droplet over a solid substrate is a key phenomenon observed in the following engineering applications: thin film coating, oil extraction, inkjet printing, and spray cooling of heated surfaces. Droplet cooling systems are known to be more effective than film or rivulet cooling systems. It is caused by the greater evaporation surface area of droplets compared with the film of the same mass and wetting surface. And the greater surface area of droplets is connected with the curvature of the interface. Location of the droplets on the cooling surface influences on the heat transfer conditions. The close distance between the droplets provides intensive heat removal, but there is a possibility of their coalescence in the liquid film. The long distance leads to overheating of the local areas of the cooling surface and the occurrence of thermal stresses. To control the location of droplets is possible by changing the roughness, structure and chemical composition of the surface. Thus, control of spreading can be implemented. The most important characteristic of spreading of droplets on solid surfaces is a dynamic contact angle, which is a function of the contact line speed or capillary number. However, there is currently no universal equation, which would describe the relationship between these parameters. This paper presents the results of the experimental studies of water droplet spreading on metal substrates with different surface roughness. The effect of the droplet growth rate and the surface roughness on spreading characteristics was studied at low capillary numbers. The shadow method using high speed video cameras recording up to 10,000 frames per seconds was implemented. A droplet profile was analyzed by Axisymmetric Drop Shape Analyses techniques. According to change of the dynamic contact angle and the contact line speed three sequential spreading stages were observed: rapid increase in the dynamic contact angle; monotonous decrease in the contact angle and the contact line speed; and form of the equilibrium contact angle at constant contact line. At low droplet growth rate, the dynamic contact angle of the droplet spreading on the surfaces with the maximum roughness is found to increase throughout the spreading time. It is due to the fact that the friction force on such surfaces is significantly greater than the inertia force; and the contact line is pinned on microasperities of a relief. At high droplet growth rate the contact angle decreases during the second stage even on the surfaces with the maximum roughness, as in this case, the liquid does not fill the microcavities, and the droplet moves over the “air cushion”, i.e. the interface is a liquid/gas/solid system. Also at such growth rates pulsation of liquid flow was detected; and the droplet oscillates during the spreading. Thus, obtained results allow to conclude that it is possible to control spreading by using the surface roughness and the growth rate of droplets on surfaces as varied factors. Also, the research findings may be used for analyzing heat transfer in rivulet and drop cooling systems of high energy equipment.

Keywords: contact line speed, droplet growth rate, dynamic contact angle, shadow system, spreading

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Authors: Elizaveta Korzhova, Sebastien Deon, Patrick Fievet, Dmitry Lopatin, Oleg Baranov

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Filtration with nanoporous ultrafiltration membranes is an attractive option to remove ionic pollutants from contaminated effluents. Unfortunately, commercial membranes are not necessarily suitable for specific applications, and their modification by polymer deposition is a fruitful way to adapt their performances accordingly. Many methods are usually used for surface modification, but a novel technique based on electrospray is proposed here. Various quantities of polymers were deposited on a commercial membrane, and the impact of the deposit is investigated on filtration performances and discussed in terms of charge and hydrophobicity. The electrospray deposition is a technique which has not been used for membrane modification up to now. It consists of spraying small drops of polymer solution under a high voltage between the needle containing the solution and the metallic support on which membrane is stuck. The advantage of this process lies in the small quantities of polymer that can be coated on the membrane surface compared with immersion technique. In this study, various quantities (from 2 to 40 μL/cm²) of solutions containing two charged polymers (13 mmol/L of monomer unit), namely polyethyleneimine (PEI) and polystyrene sulfonate (PSS), were sprayed on a negatively charged polyethersulfone membrane (PLEIADE, Orelis Environment). The efficacy of the polymer deposition was then investigated by estimating ion rejection, permeation flux, zeta-potential and contact angle before and after the polymer deposition. Firstly, contact angle (θ) measurements show that the surface hydrophilicity is notably improved by coating both PEI and PSS. Moreover, it was highlighted that the contact angle decreases monotonously with the amount of sprayed solution. Additionally, hydrophilicity enhancement was proved to be better with PSS (from 62 to 35°) than PEI (from 62 to 53°). Values of zeta-potential (ζ were estimated by measuring the streaming current generated by a pressure difference on both sides of a channel made by clamping two membranes. The ζ-values demonstrate that the deposits of PSS (negative at pH=5.5) allow an increase of the negative membrane charge, whereas the deposits of PEI (positive) lead to a positive surface charge. Zeta-potentials measurements also emphasize that the sprayed quantity has little impact on the membrane charge, except for very low quantities (2 μL/m²). The cross-flow filtration of salt solutions containing mono and divalent ions demonstrate that polymer deposition allows a strong enhancement of ion rejection. For instance, it is shown that rejection of a salt containing a divalent cation can be increased from 1 to 20 % and even to 35% by deposing 2 and 4 μL/cm² of PEI solution, respectively. This observation is coherent with the reversal of the membrane charge induced by PEI deposition. Similarly, the increase of negative charge induced by PSS deposition leads to an increase of NaCl rejection from 5 to 45 % due to electrostatic repulsion of the Cl- ion by the negative surface charge. Finally, a notable fall in the permeation flux due to the polymer layer coated at the surface was observed and the best polymer concentration in the sprayed solution remains to be determined to optimize performances.

Keywords: ultrafiltration, electrospray deposition, ion rejection, permeation flux, zeta-potential, hydrophobicity

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Authors: A. Chiker, A. Benamor, A. Haddad, Y. Hadji, M. Hadji

Abstract:

Metal matrix composites (MMCs) have been of big interest for a few decades. Their major drawback lies in their enhanced mechanical performance over unreinforced alloys. They found ground in many engineering fields, such as aeronautics, aerospace, automotive, and other structural applications. One of the most used alloys as a matrix is nickel alloys, which meet the need for high-temperature mechanical properties; some attempts have been made to develop nickel base composites reinforced by high melt point and high modulus particulates. Among the carbides used as reinforcing particulates, chromium carbide is interesting for wear applications; it is widely used as a tribological coating material in high-temperature applications requiring high wear resistance and hardness. Moreover, a set of properties make it suitable for use in MMCs, such as toughness, the good corrosion and oxidation resistance of its three polymorphs -the cubic (Cr23C6), the hexagonal (Cr7C3), and the orthorhombic (Cr3C2)-, and it’s coefficient of thermal expansion that is almost equal to that of metals. The in-situ synthesis of CrC-reinforced Ni matrix composites could be achieved by the powder metallurgy route. To ensure the in-situ reactions during the sintering process, the use of phase precursors is necessary. Recently, new precursor materials have been proposed; these materials are called MAX phases. The MAX phases are thermodynamically stable nano-laminated materials displaying unusual and sometimes unique properties. These novel phases possess Mn+1AXn chemistry, where n is 1, 2, or 3, M is an early transition metal element, A is an A-group element, and X is C or N. Herein, the pressureless sintering method is used to elaborate Ni/Cr2AlC composites. Four composites were elaborated from 5, 10, 15 and 20 wt% of Cr2AlC MAX phase precursor which fully reacted with Ni-matrix at 1100 °C sintering temperature for 4 h in argon atmosphere. XRD results showed that Cr2AlC MAX phase was totally decomposed forming chromium carbide Cr7C3, and the released Al and Cr atoms diffused in Ni matrix giving rise to γ-Ni(Al,Cr) solid solution and γ’-Ni3(Al,Cr) intermetallic. Scanning Electron Microscopy (SEM) of the elaborated samples showed the presence of nanosized Cr7C3 reinforcing particles embedded in the Ni metal matrix, which have a direct impact on the tribological properties of the composites and their hardness. All the composites exhibited higher hardness than pure Ni; whereas adding 15 wt% of Cr2AlC gives the highest hardness (1.85 GPa). Using a ball-on-disc tribometer, dry sliding tests for the elaborated composites against 100Cr6 steel ball were studied under different applied loads. The microstructures and worn surface characteristics were then analyzed using SEM and Raman spectroscopy. The results show that all the composites exhibited better wear resistance compared to pure Ni, which could be explained by the formation of a lubricious tribo-layer during sliding and the good bonding between the Ni matrix and the reinforcing phases.

Keywords: composites, microscopy, sintering, wear

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Authors: M. Zasada, A. Markiewicz, A. Erkiert-Polguj, E. Budzisz

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The epidermis is a keratinized stratified squamous epithelium covered by the hydro-lipid barrier. Therefore, active substances should be able to penetrate through this hydro-lipid coating. L-ascorbic acid is one of the vitamins which plays an important role in stimulation fibroblast to produce collagen type I and in hyperpigmentation lightening. Vitamin C is a water-soluble antioxidant, which protects skin from oxidation damage and rejuvenates photoaged skin. No-needle mesotherapy is a non-invasive rejuvenation technique depending on electric pulses, electroporation, and ultrasounds. These physicals factors result in deeper penetration of cosmetics. It is important to increase the penetration of L-ascorbic acid, thereby increasing the spectrum of its activity. The aim of the work was to assess the effectiveness of pure L-ascorbic acid activity in anti-aging therapy using a needle-free and micro-needling mesotherapy. The study was performed on a group of 35 healthy volunteers in accordance with the Declaration of Helsinki of 1964 and agreement of the Ethics Commissions no RNN/281/16/KE 2017. Women were randomized to mesotherapy or control group. Control group applied topically 2,5 ml serum containing 20% L-ascorbic acid with hydrate from strawberries, every 10 days for a period of 9 weeks. No-needle mesotherapy, on the left half of the face and micro-needling on the right with the same serum, was done in mesotherapy group. The pH of serum was 3.5-4, and the serum was prepared directly prior to the facial treatment. The skin parameters were measured at the beginning and before each treatment. The measurement of the forehead skin was done using Cutometer® (measurement of skin elasticity and firmness), Corneometer® (skin hydration measurement), Mexameter® (skin tone measurement). Also, the photographs were taken by Fotomedicus system. Additionally, the volunteers fulfilled the questionnaire. Serum was tested for microbiological purity and stability after the opening of the cosmetic. During the study, all of the volunteers were taken care of a dermatologist. The regular application of the serum has caused improvement of the skin parameters. Respectively, after 4 and 8 weeks improvement in hydration and elasticity has been seen (Corneometer®, Cutometer® results). Moreover, the number of hyper-pigmentated spots has decreased (Mexameter®). After 8 weeks the volunteers has claimed that the tested product has smoothing and moisturizing features. Subjective opinions indicted significant improvement of skin color and elasticity. The product containing the L-ascorbic acid used with intercellular penetration promoters demonstrates higher anti-aging efficiency than control. In vivo studies confirmed the effectiveness of serum and the impact of the active substance on skin firmness and elasticity, the degree of hydration and skin tone. Mesotherapy with pure L-ascorbic acid provides better diffusion of active substances through the skin.

Keywords: anti-aging, l-ascorbic acid, mesotherapy, promoters

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Authors: O. Sauperl, L. Fras Zemljic

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The textile industry is gaining increasing importance in the field of medical materials. Therefore, presented research is focused on textile materials for external (out-of-body) use. Such materials could be various hygienic textile products (diapers, tampons, sanitary napkins, incontinence products, etc.), protective textiles and various hospital linens (surgical covers, masks, gowns, cloths, bed linens, etc.) wound pillows, bandages, orthopedic socks, etc. Function of tampons and sanitary napkins is not only to provide protection during the menstrual cycle, but their function can be also to take care of physiological or pathological vaginal discharge. In general, women's intimate areas are against infection protected by a low pH value of the vaginal flora. High pH inhibits the development of harmful microorganisms, as it is difficult to be reproduced in an acidic environment. The normal vaginal flora in healthy women is highly colonized by lactobacilli. The lactic acid produced by these organisms maintains the constant acidity of the vagina. If the balance of natural protection breaks, infections can occur. In the market, there exist probiotic tampons as a medical product supplying the vagina with beneficial probiotic lactobacilli. But, many users have concerns about the use of tampons due to the possible dry-out of the vagina as well as the possible toxic shock syndrome, which is the reason that they use mainly sanitary napkins during the menstrual cycle. Functionalization of sanitary napkins with probiotics is, therefore, interesting in regard to maintain a healthy vaginal flora and to offer to users added value of the sanitary napkins in the sense of health- and environmentally-friendly products. For this reason, the presented research is oriented in functionalization of the sanitary napkins with the probiotic paste in order to activate the lactic acid bacteria presented in the core of the functionalized sanitary napkin at the time of the contact with the menstrual fluid. In this way, lactobacilli could penetrate into vagina and by maintaining healthy vaginal flora to reduce the risk of vaginal disorders. In regard to the targeted research problem, the influence of probiotic paste applied onto cotton hygienic napkins on selected properties was studied. The aim of the research was to determine whether the sanitary napkins with the applied probiotic paste may assure suitable vaginal pH to maintain a healthy vaginal flora during the use of this product. Together with this, sorption properties of probiotic functionalized sanitary napkins were evaluated and compared to the untreated one. The research itself was carried out on the basis of tracking and controlling the input parameters, currently defined by Slovenian producer (Tosama d.o.o.) as the most important. Successful functionalization of sanitary pads with the probiotic paste was confirmed by ATR-FTIR spectroscopy. Results of the methods used within the presented research show that the absorption of the pads treated with probiotic paste deteriorates compared to non-treated ones. The coating shows a 6-month stability. Functionalization of sanitary pads with probiotic paste is believed to have a commercial potential for lowering the probability of infection during the menstrual cycle.

Keywords: functionalization, probiotic paste, sanitary pads, textile materials

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Authors: Alexia Wu, Joel Ribis, Jean-Christophe Brachet, Emmanuel Clouet, Benoit Arnal, Elodie Rouesne, Stéphane Urvoy, Justine Roubaud, Yves Serruys, Frederic Lepretre

Abstract:

To enhance the safety of Light Water Reactor, accident tolerant fuel (ATF) claddings materials are under development. In the framework of CEA-AREVA-EDF collaborative program on ATF cladding materials, CEA has engaged specific studies on chromium coated zirconium alloys. Especially for Loss-of-Coolant-Accident situations, chromium coated claddings have shown some additional 'coping' time before achieving full embrittlement of the oxidized cladding, when compared to uncoated references – both tested in steam environment up to 1300°C. Nevertheless, the behavior of chromium coatings and the stability of the Zr-Cr interface under neutron irradiation remain unknown. Two main points are addressed: 1. Bulk Cr behavior under irradiation: Due to its BCC crystallographic structure, Cr is prone to Ductile-to-Brittle-Transition at quite high temperature. Irradiation could be responsible for a significant additional DBTT shift towards higher temperatures. 2. Zircaloy/Cr interface behavior under irradiation: Preliminary TEM examinations of un-irradiated samples revealed a singular Zircaloy-4/Cr interface with nanometric intermetallic phase layers. Such particular interfaces highlight questions of how they would behave under irradiation - intermetallic zirconium phases are known to be more or less stable under irradiations. Another concern is a potential enhancement of chromium diffusion into the zirconium-alpha based substrate. The purpose of this study is then to determine the behavior of such coatings after ion irradiations, as a surrogate to neutron irradiation. Ion irradiations were performed at the Jannus-Saclay facility (France). 20 MeV Kr8+ ions at 400°C with a flux of 2.8x1011 ions.cm-2.s-1 were used to irradiate chromium coatings of 1-2 µm thick on Zircaloy-4 sheets substrate. At the interface, the calculated damage is close to 10 dpa (SRIM, Quick Calculation Damage mode). Thin foil samples were prepared with FIB for both as-received and irradiated coated samples. Transmission Electron Microscopy (TEM) and in-situ tensile tests in a Scanning Electron Microscope are being used to characterize the un-irradiated and irradiated materials. High Resolution TEM highlights a great complexity of the interface before irradiation since it is formed of an alternation of intermetallic phases – C14 and C15. The interfaces formed by these intermetallic phases with chromium and zirconium show semi-coherency. Chemical analysis performed before irradiation shows some iron enrichment at the interface. The chromium coating bulk microstructures and properties are also studied before and after irradiation. On-going in-situ tensile tests focus on the capacity of chromium coatings to sustain some plastic deformation when tested up to 350°C. The stability of the Cr/Zr interface is shown after ion irradiation up to 10 dpa. This observation constitutes the first result after irradiation on these new coated claddings materials.

Keywords: accident tolerant fuel, HRTEM, interface, ion-irradiation

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