Search results for: powder X-ray diffraction

Authors: S.V. Kleyn, S.Yu. Zagorodnov, А.А. Kokoulina

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Technogenic emissions of the mining and processing complex are characterized by a high content of chemical components and solid dust particles. However, each industrial enterprise and the surrounding area have features that require refinement and parameterization. Numerous studies have shown the negative impact of fine dust PM10 and PM2.5 on the health, as well as the possibility of toxic components absorption, including heavy metals by dust particles. The target of the study was the quantitative assessment of the fractional and particle size composition of ambient air dust in the area of impact by primary magnesium production complex. Also, we tried to describe the morphology features of dust particles. Study methods. To identify the dust emission sources, the analysis of the production process has been carried out. The particulate composition of the emissions was measured using laser particle analyzer Microtrac S3500 (covered range of particle size is 20 nm to 2000 km). Particle morphology and the component composition were established by electron microscopy by scanning microscope of high resolution (magnification rate - 5 to 300 000 times) with X-ray fluorescence device S3400N ‘HITACHI’. The chemical composition was identified by X-ray analysis of the samples using an X-ray diffractometer XRD-700 ‘Shimadzu’. Determination of the dust pollution level was carried out using model calculations of emissions in the atmosphere dispersion. The calculations were verified by instrumental studies. Results of the study. The results demonstrated that the dust emissions of different technical processes are heterogeneous and fractional structure is complicated. The percentage of particle sizes up to 2.5 micrometres inclusive was ranged from 0.00 to 56.70%; particle sizes less than 10 microns inclusive – 0.00 - 85.60%; particle sizes greater than 10 microns - 14.40% -100.00%. During microscopy, the presence of nanoscale size particles has been detected. Studied dust particles are round, irregular, cubic and integral shapes. The composition of the dust includes magnesium, sodium, potassium, calcium, iron, chlorine. On the base of obtained results, it was performed the model calculations of dust emissions dispersion and establishment of the areas of fine dust РМ 10 and РМ 2.5 distribution. It was found that the dust emissions of fine powder fractions PM10 and PM2.5 are dispersed over large distances and beyond the border of the industrial site of the enterprise. The population living near the enterprise is exposed to the risk of diseases associated with dust exposure. Data are transferred to the economic entity to make decisions on the measures to minimize the risks. Exposure and risks indicators on the health are used to provide named patient health and preventive care to the citizens living in the area of negative impact of the facility.

Keywords: dust emissions, еxposure assessment, PM 10, PM 2.5

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Authors: Daniela Manila Bianchi, Samantha Lupi, Elisa Barcucci, Sandra Fragassi, Clara Tramuta, Lucia Decastelli

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Introduction: The undeclared allergens detection in food products plays a fundamental role in the safety of the allergic consumer. The protection of allergic consumers is guaranteed, in Europe, by Regulation (EU) No 1169/2011 of the European Parliament, which governs the consumer's right to information and identifies 14 food allergens to be mandatorily indicated on food labels: among these, an egg is included. An egg can be present as an ingredient or as contamination in raw and cooked products. The main allergen egg proteins are ovomucoid, ovalbumin, lysozyme, and ovotransferrin. This study presents the results of a survey conducted in Northern Italy aimed at detecting the presence of undeclared egg proteins in food matrices in the latest ten years (2011-2021). Method: In the period January 2011 - October 2021, a total of 1205 different types of food matrices (ready-to-eat, meats, and meat products, bakery and pastry products, baby foods, food supplements, pasta, fish and fish products, preparations for soups and broths) were delivered to Food Control Laboratory of Istituto Zooprofilattico Sperimentale of Piemonte Liguria and Valle d’Aosta to be analyzed as official samples in the frame of Regional Monitoring Plan of Food Safety or in the contest of food poisoning. The laboratory is ISO 17025 accredited, and since 2019, it has represented the National Reference Centre for the detection in foods of substances causing food allergies or intolerances (CreNaRiA). All samples were stored in the laboratory according to food business operator instructions and analyzed within the expiry date for the detection of undeclared egg proteins. Analyses were performed with RIDASCREEN®FAST Ei/Egg (R-Biopharm ® Italia srl) kit: the method was internally validated and accredited with a Limit of Detection (LOD) equal to 2 ppm (mg/Kg). It is a sandwich enzyme immunoassay for the quantitative analysis of whole egg powder in foods. Results: The results obtained through this study showed that egg proteins were found in 2% (n. 28) of food matrices, including meats and meat products (n. 16), fish and fish products (n. 4), bakery and pastry products (n. 4), pasta (n. 2), preparations for soups and broths (n.1) and ready-to-eat (n. 1). In particular, in 2011 egg proteins were detected in 5% of samples, in 2012 in 4%, in 2013, 2016 and 2018 in 2%, in 2014, 2015 and 2019 in 3%. No egg protein traces were detected in 2017, 2020, and 2021. Discussion: Food allergies occur in the Western World in 2% of adults and up to 8% of children. Allergy to eggs is one of the most common food allergies in the pediatrics context. The percentage of positivity obtained from this study is, however, low. The trend over the ten years has been slightly variable, with comparable data.

Keywords: allergens, food, egg proteins, immunoassay

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Authors: G. Swati, D. Haranath

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Commercially available long afterglow /persistent phosphors are proprietary materials and hence the exact composition and phase responsible for their luminescent characteristics such as initial intensity and afterglow luminescence time are not known. Further to generate various emission colors, commercially available persistence phosphors are physically blended with fluorescent organic dyes such as rodhamine, kiton and methylene blue etc. Blending phosphors with organic dyes results into complete color coverage in visible spectra, however with time, such phosphors undergo thermal and photo-bleaching. This results in the loss of their true emission color. Hence, the current work is dedicated studies on inorganic based thermally and chemically stable primary color emitting nanophosphors namely SrAl2O4:Eu2+, Dy3+, (CaZn)TiO3:Pr3+, and Sr2MgSi2O7:Eu2+, Dy3+. SrAl2O4: Eu2+, Dy3+ phosphor exhibits a strong excitation in UV and visible region (280-470 nm) with a broad emission peak centered at 514 nm is the characteristic emission of parity allowed 4f65d1→4f7 transitions of Eu2+ (8S7/2→2D5/2). Sunlight excitable Sr2MgSi2O7:Eu2+,Dy3+ nanophosphors emits blue color (464 nm) with Commercial international de I’Eclairage (CIE) coordinates to be (0.15, 0.13) with a color purity of 74 % with afterglow time of > 5 hours for dark adapted human eyes. (CaZn)TiO3:Pr3+ phosphor system possess high color purity (98%) which emits intense, stable and narrow red emission at 612 nm due intra 4f transitions (1D2 → 3H4) with afterglow time of 0.5 hour. Unusual property of persistence luminescence of these nanophoshphors supersedes background effects without losing sensitive information these nanophosphors offer several advantages of visible light excitation, negligible substrate interference, high contrast bifurcation of ridge pattern, non-toxic nature revealing finger ridge details of the fingerprints. Both level 1 and level 2 features from a fingerprint can be studied which are useful for used classification, indexing, comparison and personal identification. facile methodology to extract high contrast fingerprints on non-porous and porous substrates using a chemically inert, visible light excitable, and nanosized phosphorescent label in the dark has been presented. The chemistry of non-covalent physisorption interaction between the long afterglow phosphor powder and sweat residue in fingerprints has been discussed in detail. Real-time fingerprint development on porous and non-porous substrates has also been performed. To conclude, apart from conventional dark vision applications, as prepared primary color emitting afterglow phosphors are potentional candidate for developing high contrast latent fingerprints.

Keywords: fingerprints, luminescence, persistent phosphors, rare earth

Procedia PDF Downloads 218

Authors: Malkhaz Jokhadze, Vakhtang Mshvildadze, Levan Makaradze, Ekaterine Mosidze, Salome Barbaqadze, Mariam Murtazashvili, Dali Berashvili, Koba sivsivadze, Lasha Bakuridze, Aliosha Bakuridze

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Essential oils are one of the most important groups of biologically active substances present in plants. Due to the chemical diversity of components, essential oils and their preparations have a wide spectrum of pharmacological action. They have bactericidal, antiviral, fungicidal, antiprotozoal, anti-inflammatory, spasmolytic, sedative and other activities. They are expectorant, spasmolytic, sedative, hypotensive, secretion enhancing, antioxidant remedies. Based on preliminary pharmacological studies, we have developed a formulation called “Phytobiotic” containing essential oils, a feed additive for poultry as an alternative to antibiotics. Phytobiotic is a water-soluble powder containing a composition of essential oils of thyme, clary, monarda and auxiliary substances: dry extract of liquorice and inhalation lactose. On this stage of research, the goal was to study the chemical composition of provided phytobiotic, identify the main substances and determine their quantity, investigate the biological activity of phytobiotic through in vitro and in vivo studies. Using gas chromatography-mass spectrometry, 38 components were identified in phytobiotic, representing acyclic-, monocyclic-, bicyclic-, and sesquiterpenes. Together with identification of main active substances, their quantitative content was determined, including acyclic terpene alcohol β-linalool, acyclic terpene ketone linalyl acetate, monocyclic terpenes: D-limonene and γ-terpinene, monocyclic aromatic terpene thymol. Provided phytobiotic has pronounced and at the same time broad spectrum of antibacterial activity. In the cell model, phytobiotic showed weak antioxidant activity, and it was stronger in the ORAC (chemical model) tests. Meanwhile anti-inflammatory activity was also observed. When fowls were supplied feed enriched with phytobiotic, it was observed that gained weight of the chickens in the experimental group exceeded the same data for the control group during the entire period of the experiment. The survival rate of broilers in the experimental group during the growth period was 98% compared to -94% in the control group. As a result of conducted researches probable four different mechanisms which are important for the action of phytobiotics were identified: sensory, metabolic, antioxidant and antibacterial action. General toxic, possible local irritant and allergenic effects of phytobiotic were also investigated. Performed assays proved that formulation is safe.

Keywords: clary, essential oils, monarda, poultry, phytobiotics, thyme

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Authors: Drago Diaz Aleman, Jose Luis Saorin Perez, Cecile Meier, Itahisa Perez Conesa, Jorge De La Torre Cantero

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Traditional manufacturing techniques used in artistic contexts compete with highly productive and efficient industrial procedures. The craft techniques and associated business models tend to disappear under the pressure of the appearance of mass-produced products that compete in all niche markets, including those traditionally reserved for the work of art. The surplus value derived from the prestige of the author, the exclusivity of the product or the mastery of the artist, do not seem to be sufficient reasons to preserve this productive model. In the last years, the adoption of open source digital manufacturing technologies in small art workshops can favor their permanence by assuming great advantages such as easy accessibility, low cost, and free modification, adapting to specific needs of each workshop. It is possible to use pieces modeled by computer and made with FDM (Fused Deposition Modeling) 3D printers that use PLA (polylactic acid) in the procedures of artistic casting. Models printed by PLA are limited to approximate minimum sizes of 3 cm, and optimal layer height resolution is 0.1 mm. Due to these limitations, it is not the most suitable technology for artistic casting processes of smaller pieces. An alternative to solve size limitation, are printers from the type (SLS) "selective sintering by laser". And other possibility is a laser hardens, by layers, metal powder and called DMLS (Direct Metal Laser Sintering). However, due to its high cost, it is a technology that is difficult to introduce in small artistic foundries. The low-cost DLP (Digital Light Processing) type printers can offer high resolutions for a reasonable cost (around 0.02 mm on the Z axis and 0.04 mm on the X and Y axes), and can print models with castable resins that allow the subsequent direct artistic casting in precious metals or their adaptation to processes such as electroforming. In this work, the design of a DLP 3D printer is detailed, using backlit LCD screens with ultraviolet light. Its development is totally "open source" and is proposed as a kit made up of electronic components, based on Arduino and easy to access mechanical components in the market. The CAD files of its components can be manufactured in low-cost FDM 3D printers. The result is less than 500 Euros, high resolution and open-design with free access that allows not only its manufacture but also its improvement. In future works, we intend to carry out different comparative analyzes, which allow us to accurately estimate the print quality, as well as the real cost of the artistic works made with it.

Keywords: traditional artistic techniques, DLP 3D printer, artistic casting, electroforming

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Authors: Belen Montero, Carmen Ramirez, Maite Rico, Rebeca Bouza, Irene Derungs

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Starch is a promising polymer for producing biocomposite materials because it is renewable, completely biodegradable and easily available at a low cost. Thermoplastic starches (TPS) can be obtained after the disruption and plasticization of native starch with a plasticizer. In this work, the solvent casting method was used to obtain TPS films from wheat starch plasticized with glycerol and reinforced with nanocellulose (CNC). X-ray diffraction analysis was used to follow the evolution of the crystallinity. The native wheat starch granules have shown a profile corresponding to A-type crystal structures typical for cereal starches. When TPS films are analyzed a high amorphous halo centered on 19º is obtained, indicating the plasticization process is completed. SEM imaging was made in order to analyse the morphology. The image from the raw wheat starch granules shows a bimodal granule size distribution with some granules in large round disk-shape forms (A-type) and the others as smaller spherical particles (B-type). The image from the neat TPS surface shows a continuous surface. No starch aggregates or swollen granules can be seen so, the plasticization process is complete. In the surfaces of reinforced TPS films aggregates are seen as the CNC concentration in the matrix increases. The CNC influence on the mechanical properties of TPS films has been studied by dynamic mechanical analysis. A direct relation exists between the storage modulus values, E’, and the CNC content in reinforced TPS films: higher is the content of nanocellulose in the composite, higher is the value of E’. This reinforcement effect can be explained by the appearance of a strong and crystalline nanoparticle-TPS interphase. Thermal stability of films was analysed by TGA. It has not observed any influence on the behaviour related to the thermal degradation of films with the incorporation of the CNC. Finally, the resistance to the water absorption films was analysed following the standard UNE-EN ISO 1998:483. The percentage of water absorbed by the samples at each time was calculated. The addition of 5 wt % of CNC to the TPS matrix leads to a significant improvement in the moisture resistance of the starch based material decreasing their diffusivity. It has been associated to the formation of a nanocrystal network that prevents swelling of the starch and therefore water absorption and to the high crystallinity of cellulose compared to starch. As a conclusion, the wheat film reinforced with 5 wt % of cellulose nanocrystals seems to be a good alternative for short-life applications into the packaging industry, because of its greatest rigidity, thermal stability and moisture sorption resistance.

Keywords: biocomposites, nanocellulose, starch, wheat

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Authors: M. S. Stepanova, V. V. Zakharov, P. D. Khavlyuk, I. D. Skurlov, A. Y. Dubovik, A. L. Rogach

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Carbon dots are small carbon-based spherical nanoparticles, which are typically less than 10 nm in size that can be modified with surface passivation and heteroatoms doping. The light-absorbing ability of carbon dots has attracted a significant amount of attention in photoluminescence for bioimaging and fluorescence sensing applications owing to their advantages, such as tunable fluorescence emission, photo- and thermostability and low toxicity. In this study, carbon dots were synthesized by the solvothermal method from citric acid and ethylenediamine dissolved in water. The solution was heated for 5 hours at 200°C and then cooled down to room temperature. The carbon dots films were obtained by evaporation from a high-concentration aqueous solution. The increase of both luminescence intensity and light transmission was obtained as a result of a 405 nm laser exposure to a part of the carbon dots film, which was detected using a confocal laser scanning microscope (LSM 710, Zeiss). Blueshift up to 35 nm of the luminescence spectrum is observed as luminescence intensity, which is increased more than twofold. The exact value of the shift depends on the time of the laser exposure. This shift can be caused by the modification of surface groups at the carbon dots, which are responsible for long-wavelength luminescence. In addition, a shift of the absorption peak by 10 nm and a decrease in the optical density at the wavelength of 350 nm is detected, which is responsible for the absorption of surface groups. The obtained sample was also studied with time-resolved confocal fluorescence microscope (MicroTime 100, PicoQuant), which made it possible to receive a time-resolved photoluminescence image and construct emission decays of the laser-exposed and non-exposed areas. 5 MHz pulse rate impulse laser has been used as a photoluminescence excitation source. Photoluminescence decay was approximated by two exhibitors. The laser-exposed area has the amplitude of the first-lifetime component (A1) twice as much as before, with increasing τ1. At the same time, the second-lifetime component (A2) decreases. These changes evidence a modification of the surface groups of carbon dots. The detected effect can be used to create thermostable fluorescent marks, the physical size of which is bounded by the diffraction limit of the optics (~ 200-300 nm) used for exposure and to improve the optical properties of carbon dots or in the field of optical encryption. Acknowledgements: This work was supported by the Ministry of Science and Higher Education of Russian Federation, goszadanie no. 2019-1080 and financially supported by Government of Russian Federation, Grant 08-08.

Keywords: carbon dots, photoactivation, optical properties, photoluminescence and absorption spectra

Procedia PDF Downloads 162

Authors: Loveline Ambo Angwah

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The processing of cassava from tubers or roots into food using crude and rudimentary method (hand peeling, grating, frying and to sun drying) is a very cumbersome and difficult process. The crude methods are time consuming and labour intensive. While on the other hand, modern processing method, that is using machines to perform the various processes as washing, peeling, grinding, oven drying, fermentation and frying is easier, less time consuming, and less labour intensive. Rudimentarily, cassava roots are processed into numerous products and utilized in various ways according to local customs and preferences. For the people of Ngwo village, cassava is transformed locally into flour or powder form called ‘cumcum’. It is also sucked into water to give a kind of food call ‘water fufu’ and fried to give ‘garri’. The leaves are consumed as vegetables. Added to these, its relative high yields; ability to stay underground after maturity for long periods give cassava considerable advantage as a commodity that is being used by poor rural folks in the community, to fight poverty. It plays a major role in efforts to alleviate the food crisis because of its efficient production of food energy, year-round availability, tolerance to extreme stress conditions, and suitability to present farming and food systems in Africa. Improvement of cassava processing and utilization techniques would greatly increase labor efficiency, incomes, and living standards of cassava farmers and the rural poor, as well as enhance the-shelf life of products, facilitate their transportation, increase marketing opportunities, and help improve human and livestock nutrition. This paper presents a general overview of crude ways in cassava processing and utilization methods now used by subsistence and small-scale farmers in Ngwo village of the North West region in Cameroon, and examine the opportunities of improving processing technologies. Cassava needs processing because the roots cannot be stored for long because they rot within 3-4 days of harvest. They are bulky with about 70% moisture content, and therefore transportation of the tubers to markets is difficult and expensive. The roots and leaves contain varying amounts of cyanide which is toxic to humans and animals, while the raw cassava roots and uncooked leaves are not palatable. Therefore, cassava must be processed into various forms in order to increase the shelf life of the products, facilitate transportation and marketing, reduce cyanide content and improve palatability.

Keywords: cassava roots, crude ways, food system, poverty

Procedia PDF Downloads 166

Authors: Evrim Colak, Andriy E. Serebryannikov, Pavel V. Usik, Ekmel Ozbay

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Working with a dielectric photonic crystal (PC) structure which does not include surface corrugations, unidirectional transmission and dual-beam splitting are observed under normal incidence as a result of the strong diffractions caused by the embedded defect layer. The defect layer has twice the period of the regular PC segments which sandwich the defect layer. Although the PC has even number of rows, the structural symmetry is broken due to the asymmetric placement of the defect layer with respect to the symmetry axis of the regular PC. The simulations verify that efficient splitting and occurrence of strong diffractions are related to the dispersion properties of the Floquet-Bloch modes of the photonic crystal. Unidirectional and bi-directional splitting, which are associated with asymmetric transmission, arise due to the dominant contribution of the first positive and first negative diffraction orders. The effect of the depth of the defect layer is examined by placing single defect layer in varying rows, preserving the asymmetry of PC. Even for deeply buried defect layer, asymmetric transmission is still valid even if the zeroth order is not coupled. This transmission is due to evanescent waves which reach to the deeply embedded defect layer and couple to higher order modes. In an additional selected performance, whichever surface is illuminated, i.e., in both upper and lower surface illumination cases, incident beam is split into two beams of equal intensity at the output surface where the intensity of the out-going beams are equal for both illumination cases. That is, although the structure is asymmetric, symmetric bidirectional transmission with equal transmission values is demonstrated and the structure mimics the behavior of symmetric structures. Finally, simulation studies including the examination of a coupled-cavity defect for two different permittivity values (close to the permittivity values of GaAs or Si and alumina) reveal unidirectional splitting for a wider band of operation in comparison to the bandwidth obtained in the case of a single embedded defect layer. Since the dielectric materials that are utilized are low-loss and weakly dispersive in a wide frequency range including microwave and optical frequencies, the studied structures should be scalable to the mentioned ranges.

Keywords: asymmetric transmission, beam deflection, blazing, bi-directional splitting, defect layer, dual beam splitting, Floquet-Bloch modes, isofrequency contours, line defect, oblique incidence, photonic crystal, unidirectionality

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Authors: Raj Kumar, Prem Felix Siril

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The poor aqueous solubility of many pharmaceutical drugs and potential drug candidates is a big challenge in drug development. Nanoformulation of such candidates is one of the major solutions for the delivery of such drugs. We initially developed the evaporation assisted solvent-antisolvent interaction (EASAI) method. EASAI method is use full to prepared nanoparticles of poor water soluble drugs with spherical morphology and particles size below 100 nm. However, to further improve the effect formulation to reduce number of dose and side effect it is important to control the delivery of drugs. However, many drug delivery systems are available. Among the many nano-drug carrier systems, solid lipid nanoparticles (SLNs) have many advantages over the others such as high biocompatibility, stability, non-toxicity and ability to achieve controlled release of drugs and drug targeting. SLNs can be administered through all existing routes due to high biocompatibility of lipids. SLNs are usually composed of lipid, surfactant and drug were encapsulated in lipid matrix. A number of non-steroidal anti-inflammatory drugs (NSAIDs) have poor bioavailability resulting from their poor aqueous solubility. In the present work, SLNs loaded with NSAIDs such as Nabumetone (NBT), Ketoprofen (KP) and Ibuprofen (IBP) were successfully prepared using different lipids and surfactants. We studied and optimized experimental parameters using a number of lipids, surfactants and NSAIDs. The effect of different experimental parameters such as lipid to surfactant ratio, volume of water, temperature, drug concentration and sonication time on the particles size of SLNs during the preparation using hot-melt sonication was studied. It was found that particles size was directly proportional to drug concentration and inversely proportional to surfactant concentration, volume of water added and temperature of water. SLNs prepared at optimized condition were characterized thoroughly by using different techniques such as dynamic light scattering (DLS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and differential scanning calorimetry and Fourier transform infrared spectroscopy (FTIR). We successfully prepared the SLN of below 220 nm using different lipids and surfactants combination. The drugs KP, NBT and IBP showed 74%, 69% and 53% percentage of entrapment efficiency with drug loading of 2%, 7% and 6% respectively in SLNs of Campul GMS 50K and Gelucire 50/13. In-vitro drug release profile of drug loaded SLNs is shown that nearly 100% of drug was release in 6 h.

Keywords: nanoparticles, delivery, solid lipid nanoparticles, hot-melt sonication, poor water soluble drugs, solubility, bioavailability

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Authors: Michalina Aniola, Andrzej Katrusiak

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4,4-Bipyridine is an important compound often used in chemical practice and more recently frequently applied for designing new metal organic framework (MoFs). Here we present a systematic high-pressure study of its hydrobromide salt. 4,4-Bipyridine hydrobromide monohydrate, 44biPyHBrH₂O, at ambient-pressure is orthorhombic, space group P212121 (phase a). Its hydrostatic compression shows that it is stable to 1.32 GPa at least. However, the recrystallization above 0.55 GPa reveals a new hidden b-phase (monoclinic, P21/c). Moreover, when the 44biPyHBrH2O is heated to high temperature the chemical reactions of this compound in methanol solution can be observed. High-pressure experiments were performed using a Merrill-Bassett diamond-anvil cell (DAC), modified by mounting the anvils directly on the steel supports, and X-ray diffraction measurements were carried out on a KUMA and Excalibur diffractometer equipped with an EOS CCD detector. At elevated pressure, the crystal of 44biPyHBrH₂O exhibits several striking and unexpected features. No signs of instability of phase a were detected to 1.32 GPa, while phase b becomes stable at above 0.55 GPa, as evidenced by its recrystallizations. Phases a and b of 44biPyHBrH2O are partly isostructural: their unit-cell dimensions and the arrangement of ions and water molecules are similar. In phase b the HOH-Br- chains double the frequency of their zigzag motifs, compared to phase a, and the 44biPyH+ cations change their conformation. Like in all monosalts of 44biPy determined so far, in phase a the pyridine rings are twisted by about 30 degrees about bond C4-C4 and in phase b they assume energy-unfavorable planar conformation. Another unusual feature of 44biPyHBrH2O is that all unit-cell parameters become longer on the transition from phase a to phase b. Thus the volume drop on the transition to high-pressure phase b totally depends on the shear strain of the lattice. Higher temperature triggers chemical reactions of 44biPyHBrH2O with methanol. When the saturated methanol solution compound precipitated at 0.1 GPa and temperature of 423 K was required to dissolve all the sample, the subsequent slow recrystallization at isochoric conditions resulted in disalt 4,4-bipyridinium dibromide. For the 44biPyHBrH2O sample sealed in the DAC at 0.35 GPa, then dissolved at isochoric conditions at 473 K and recrystallized by slow controlled cooling, a reaction of N,N-dimethylation took place. It is characteristic that in both high-pressure reactions of 44biPyHBrH₂O the unsolvated disalt products were formed and that free base 44biPy and H₂O remained in the solution. The observed reactions indicate that high pressure destabilized ambient-pressure salts and favors new products. Further studies on pressure-induced reactions are carried out in order to better understand the structural preferences induced by pressure.

Keywords: conformation, high-pressure, negative area compressibility, polymorphism

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Authors: Lucie Speyer, Vincent Lecocq, Séverine Humbert, Antoine Hugon

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Mesoporous alumina is commonly used as a catalyst support for the hydrotreating of heavy petroleum cuts. The process of fabrication usually involves: the synthesis of the boehmite AlOOH precursor, a kneading-extrusion step, and a calcination in order to obtain the final alumina extrudates. Alumina is described as a complex porous medium, generally agglomerates constituted of aggregated nanocrystallites. Its porous texture directly influences the active phase deposition and mass transfer, and the catalytic properties. Then, it is easy to figure out that each step of the fabrication of the supports has a role on the building of their porous network, and has to be well understood to optimize the process. The synthesis of boehmite by precipitation of aluminum salts was extensively studied in the literature and the effect of various parameters, such as temperature or pH, are known to influence the size and shape of the crystallites and the specific surface area of the support. The calcination step, through the topotactic transition from boehmite to alumina, determines the final properties of the support and can tune the surface area, pore volume and pore diameters from those of boehmite. However, the kneading extrusion step has been subject to a very few studies. It generally consists in two steps: an acid, then a basic kneading, where the boehmite powder is introduced in a mixer and successively added with an acid and a base solution to form an extrudable paste. During the acid kneading, the induced positive charges on the hydroxyl surface groups of boehmite create an electrostatic repulsion which tends to separate the aggregates and even, following the conditions, the crystallites. The basic kneading, by reducing the surface charges, leads to a flocculation phenomenon and can control the reforming of the overall structure. The separation and reassembling of the particles constituting the boehmite paste have a quite obvious influence on the textural properties of the material. In this work, we are focused on the influence of the kneading step on the alumina catalysts supports. Starting from an industrial boehmite, extrudates are prepared using various kneading conditions. The samples are studied by nitrogen physisorption in order to analyze the evolution of the textural properties, and by synchrotron small-angle X-ray scattering (SAXS), a more original method which brings information about agglomeration and aggregation of the samples. The coupling of physisorption and SAXS enables a precise description of the samples, as same as an accurate monitoring of their evolution as a function of the kneading conditions. These ones are found to have a strong influence of the pore volume and pore size distribution of the supports. A mechanism of evolution of the texture during the kneading step is proposed and could be attractive in order to optimize the texture of the supports and then, their catalytic performances.

Keywords: alumina catalyst support, kneading, nitrogen physisorption, small-angle X-ray scattering

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Authors: Paula Quiterio, Arlete Apolinario, Celia T. Sousa, Joao Azevedo, Paula Dias, Adelio Mendes, Joao P. Araujo

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Nowadays one of the mankind's greatest challenges has been the supply of low-cost and environmentally friendly energy sources as an alternative to non-renewable fossil fuels. Hydrogen has been considered a promising solution, representing a clean and low-cost fuel. It can be produced directly from clean and abundant resources, such as sunlight and water, using photoelectrochemical cells (PECs), in a process that mimics the nature´s photosynthesis. Hematite (alpha-Fe2O3) has attracted considerable attention as a promising photoanode for solar water splitting, due to its high chemical stability, nontoxicity, availability and low band gap (2.2 eV), which allows reaching a high thermodynamic solar-to-hydrogen efficiency of 16.8 %. However, the main drawbacks of hematite such as the short hole diffusion length and the poor conductivity that lead to high electron-hole recombination result in significant PEC efficiency losses. One strategy to overcome these limitations and to increase the PEC efficiency is to use 1D nanostructures, such as nanotubes (NTs) and nanowires (NWs), which present high aspect ratios and large surface areas providing direct pathways for electron transport up to the charge collector and minimizing the recombination losses. In particular, due to the ultrathin walls of the NTs, the holes can reach the surface faster than in other nanostructures, representing a key factor for the NTs photoresponse. In this work, we prepared hematite NWs and NTs, respectively by hydrothermal process and electrochemical anodization. For hematite NWs growing, we studied the effect of variable hydrothermal conditions, different annealing temperatures and time, and the use of Ti and Sn dopants on the morphology and PEC performance. The crystalline phase characterization by X-ray diffraction was crucial to distinguish the formation of hematite and other iron oxide phases, alongside its effect on the photoanodes conductivity and consequent PEC efficiency. The conductivity of the as-prepared NWs is very low, in the order of 10-5 S cm-1, but after doping and annealing optimization it increased by a factor of 105. A high photocurrent density of 1.02 mA cm-2 at 1.45 VRHE was obtained under simulated sunlight, which is a very promising value for this kind of hematite nanostructures. The stability of the photoelectrodes was also tested, presenting good stability after several J-V measurements over time. The NTs, synthesized by fast anodizations with potentials ranging from 20-100 V, presented a linear growth of the NTs pore walls, with very low thicknesses from 10 - 18 nm. These preliminary results are also very promising for the use of hematite photoelectrodes on PEC hydrogen applications.

Keywords: hematite, nanotubes, nanowires, photoelectrochemical cells

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Authors: Ampe Mohottige Sachinthi Sandaruwani Amarasiri, Anoja Priyadarshani Attanayake, Kamani Ayoma Perera Wijewardana Jayatilaka, Lakmini Kumari Boralugoda Mudduwa

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The search for alternative pharmacological therapies based on natural extracts for renal failure has become an urgent need, due to paucity of effective pharmacotherapy. The current study was undertaken to evaluate the acute nephroprotective effect of aqueous leaf extract of Plectranthus amboinicus (Roxb.) (Family: Lamiaceae), a medicinal plant used in traditional Ayurvedic medicine for the management of renal diseases in Sri Lanka. The study was performed in adriamycin (ADR) induced nephrotoxic in Wistar rats. Wistar rats were randomly divided into four groups each with six rats. A single dose of ADR (20 mg/kg body wt., ip) was used for the induction of nephrotoxicity in all groups of rats except group one. The treatments were started 24 hours after induction of nephrotoxicity and continued for three days. Group one and two served as healthy and nephrotoxic control rats and were administered equivalent volumes of normal saline (0.9% NaCl) orally. Group three and four nephrotoxic rats were administered the lyophilized powder of the aqueous extract of P. amboinicus (400 mg/ kg body wt.; equivalent human therapeutic dose) and the standard drug, fosinopril sodium (0.09 mg/ kg body wt.) respectively. Urine and blood samples were collected from rats in each group at the end of the period of intervention for the estimation of selected renal parameters. H and E stained sections of the kidney tissues were examined for histopathological changes. Rats treated with the plant extract showed significant improvement in biochemical parameters and histopathological changes compared to ADR induced nephrotoxic group. The elevation of serum concentrations of creatinine and β2-microglobulin were decreased by 38%, and 66% in plant extract treated nephrotoxic rats respectively (p < 0.05). In addition, serum concentrations of total protein and albumin were significantly increased by 25% and 14% in rats treated with P. amboinicus respectively (p < 0.05). The results of β2 –microglobulin and serum total protein demonstrated a significant reduction in the elevated values in rats administered with the plant extract (400 mg/kg) compared to that of fosinopril (0.09 mg/kg). Urinary protein loss in 24hr urine samples was significantly decreased in rats treated with both fosinopril (86%) and P. ambonicus (56%) at the end of the intervention (p < 0.01). Accordingly, an attenuation of morphological destruction was observed in the H and E stained sections of the kidney with the treatments of plant extract and fosinopril. The results of the present study revealed that the aqueous leaf extract of P. amboinicus possesses significant nephroprotective activity at the equivalent therapeutic dose of 400 mg/ kg against adriamycin induced acute nephrotoxicity.

Keywords: biochemical assessment, histopathological assessment, nephroprotective activity, Plectranthus amboinicus

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Authors: Osman Adiguzel

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Shape memory effect is a peculiar property exhibited by certain alloy systems and based on martensitic transformation, and shape memory properties are closely related to the microstructures of the material. Shape memory effect is linked with martensitic transformation, which is a solid state phase transformation and occurs with the cooperative movement of atoms by means of lattice invariant shears on cooling from high-temperature parent phase. Lattice twinning and detwinning can be considered as elementary processes activated during the transformation. Thermally induced martensite occurs as martensite variants, in self-accommodating manner and consists of lattice twins. Also, this martensite is called the twinned martensite or multivariant martensite. Deformation of shape memory alloys in martensitic state proceeds through a martensite variant reorientation. The martensite variants turn into the reoriented single variants with deformation, and the reorientation process has great importance for the shape memory behavior. Copper based alloys exhibit this property in metastable β- phase region, which has DO3 –type ordered lattice in ternary case at high temperature, and these structures martensiticaly turn into the layered complex structures with lattice twinning mechanism, on cooling from high temperature parent phase region. The twinning occurs as martensite variants with lattice invariant shears in two opposite directions, <110 > -type directions on the {110}- type plane of austenite matrix. Lattice invariant shear is not uniform in copper based ternary alloys and gives rise to the formation of unusual layered structures, like 3R, 9R, or 18R depending on the stacking sequences on the close-packed planes of the ordered lattice. The unit cell and periodicity are completed through 18 atomic layers in case of 18R-structure. On the other hand, the deformed material recovers the original shape on heating above the austenite finish temperature. Meanwhile, the material returns to the twinned martensite structures (thermally induced martensite structure) in one way (irreversible) shape memory effect on cooling below the martensite finish temperature, whereas the material returns to the detwinned martensite structure (deformed martensite) in two-way (reversible) shape memory effect. Shortly one can say that the microstructural mechanisms, responsible for the shape memory effect are the twinning and detwinning processes as well as martensitic transformation. In the present contribution, x-ray diffraction, transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) studies were carried out on two copper-based ternary alloys, CuZnAl, and CuAlMn.

Keywords: shape memory effect, martensitic transformation, twinning and detwinning, layered structures

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Authors: M. Shahin Alam, Satoru Takahashi, Mariko Itoh, Miyuki Komura, Mayuko Suzuki, Natthanan Sangsriratanakul, Kazuaki Takehara

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Cleaning and disinfection are key components of routine biosecurity in livestock farming and food processing industry. The usage of suitable disinfectants and their proper concentration are important factors for a successful biosecurity program. Disinfectants have optimum bactericidal and virucidal efficacies at temperatures above 20°C, but very few studies on application and effectiveness of disinfectants at low temperatures have been done. In the present study, the bactericidal efficacies of food additive grade calcium hydroxide (FdCa(OH)), quaternary ammonium compound (QAC) and their mixture, were investigated under different conditions, including time, organic materials (fetal bovine serum: FBS) and temperature, either in suspension or in carrier test. Salmonella Infantis and Escherichia coli, which are the most prevalent gram negative bacteria in commercial poultry housing and food processing industry, were used in this study. Initially, we evaluated these disinfectants at two different temperatures (4°C and room temperature (RT) (25°C ± 2°C)) and 7 contact times (0, 5 and 30 sec, 1, 3, 20 and 30 min), with suspension tests either in the presence or absence of 5% FBS. Secondly, we investigated the bactericidal efficacies of these disinfectants by carrier tests (rubber, stainless steel and plastic) at same temperatures and 4 contact times (30 sec, 1, 3, and 5 min). Then, we compared the bactericidal efficacies of each disinfectant within their mixtures, as follows. When QAC was diluted with redistilled water (dW2) at 1: 500 (QACx500) to obtain the final concentration of didecyl-dimethylammonium chloride (DDAC) of 200 ppm, it could inactivate Salmonella Infantis within 5 sec at RT either with or without 5% FBS in suspension test; however, at 4°C it required 30 min in presence of 5% FBS. FdCa(OH)2 solution alone could inactivate bacteria within 1 min both at RT and 4°C even with 5% FBS. While FdCa(OH)2 powder was added at final concentration 0.2% to QACx500 (Mix500), the mixture could inactivate bacteria within 30 sec and 5 sec, respectively, with or without 5% FBS at 4°C. The findings from the suspension test indicated that low temperature inhibited the bactericidal efficacy of QAC, whereas Mix500 was effective, regardless of short contact time and low temperature, even with 5% FBS. In the carrier test, single disinfectant required bit more time to inactivate bacteria on rubber and plastic surfaces than on stainless steel. However, Mix500 could inactivate S. Infantis on rubber, stainless steel and plastic surfaces within 30 sec and 1 min, respectively, at RT and 4°C; but, for E. coli, it required only 30 sec at both temperatures. So, synergistic effects were observed on different carriers at both temperatures. For a successful enhancement of biosecurity during winter, the disinfectants should be selected that could have short contact times with optimum efficacy against the target pathogen. The present study findings help farmers to make proper strategies for application of disinfectants in their livestock farming and food processing industry.

Keywords: carrier, food additive grade calcium hydroxide (FdCa(OH)₂), quaternary ammonium compound, synergistic effects

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Authors: Almaz R. Gazizov, Sergey S. Kharintsev, Myakzyum Kh. Salakhov

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This work deals with background signal suppression in tip-enhanced near-field optical microscopy (TENOM). The background appears because an optical signal is detected not only from the subwavelength area beneath the tip but also from a wider diffraction-limited area of laser’s waist that might contain another substance. The background can be reduced by using a taper probe with a grating on its lateral surface where an external illumination causes surface plasmon excitation. It requires the grating with parameters perfectly matched with a given incident light for effective light coupling. This work is devoted to an analysis of the light-grating coupling and a quest of grating parameters to enhance a near-field light beneath the tip apex. The aim of this work is to find the figure of merit of plasmon excitation depending on grating period and location of grating in respect to the apex. In our consideration the metallic grating on the lateral surface of the tapered plasmonic probe is illuminated by a plane wave, the electric field is perpendicular to the sample surface. Theoretical model of efficiency of plasmon excitation and propagation toward the apex is tested by fdtd-based numerical simulation. An electric field of the incident light is enhanced on the grating by every single slit due to lightning rod effect. Hence, grating causes amplitude and phase modulation of the incident field in various ways depending on geometry and material of grating. The phase-modulating grating on the probe is a sort of metasurface that provides manipulation by spatial frequencies of the incident field. The spatial frequency-dependent electric field is found from the angular spectrum decomposition. If one of the components satisfies the phase-matching condition then one can readily calculate the figure of merit of plasmon excitation, defined as a ratio of the intensities of the surface mode and the incident light. During propagation towards the apex, surface wave undergoes losses in probe material, radiation losses, and mode compression. There is an optimal location of the grating in respect to the apex. One finds the value by matching quadratic law of mode compression and the exponential law of light extinction. Finally, performed theoretical analysis and numerical simulations of plasmon excitation demonstrate that various surface waves can be effectively excited by using the overtones of a period of the grating or by phase modulation of the incident field. The gratings with such periods are easy to fabricate. Tapered probe with the grating effectively enhances and localizes the incident field at the sample.

Keywords: angular spectrum decomposition, efficiency, grating, surface plasmon, taper nanoantenna

Procedia PDF Downloads 282

Authors: Qian Li, Zhaoping Zhong

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Sewage sludge, a typical solid waste, has inevitably been produced in enormous quantities in China. Still worse, the amount of sewage sludge produced has been increasing due to rapid economic development and urbanization. Compared to the conventional method to treat sewage sludge, pyrolysis has been considered an economic and ecological technology because it can significantly reduce the sludge volume, completely kill pathogens, and produce valuable solid, gas, and liquid products. However, the large-scale utilization of sludge biochar has been limited due to the considerable risk posed by heavy metals in the sludge. Heavy metals enriched in pyrolytic biochar could be divided into exchangeable, reducible, oxidizable, and residual forms. The residual form of heavy metals is the most stable and cannot be used by organisms. Kaolin and zeolite are environmentally friendly inorganic minerals with a high surface area and heat resistance characteristics. So, they exhibit the enormous potential to immobilize heavy metals. In order to reduce the risk of leaching heavy metals in the pyrolysis biochar, this study pyrolyzed sewage sludge mixed with kaolin/zeolite in a small rotary kiln. The influences of additives and pyrolysis temperature on the leaching concentration and morphological transformation of heavy metals in pyrolysis biochar were investigated. The potential mechanism of stabilizing heavy metals in the co-pyrolysis of sludge blended with kaolin/zeolite was explained by scanning electron microscopy, X-ray diffraction, and specific surface area and porosity analysis. The European Community Bureau of Reference sequential extraction procedure has been applied to analyze the forms of heavy metals in sludge and pyrolysis biochar. All the concentrations of heavy metals were examined by flame atomic absorption spectrophotometry. Compared with the proportions of heavy metals associated with the F4 fraction in pyrolytic carbon prepared without additional agents, those in carbon obtained by co-pyrolysis of sludge and kaolin/zeolite increased. Increasing the additive dosage could improve the proportions of the stable fraction of various heavy metals in biochar. Kaolin exhibited a better effect on stabilizing heavy metals than zeolite. Aluminosilicate additives with excellent adsorption performance could capture more released heavy metals during sludge pyrolysis. Then heavy metal ions would react with the oxygen ions of additives to form silicate and aluminate, causing the conversion of heavy metals from unstable fractions (sulfate, chloride, etc.) to stable fractions (silicate, aluminate, etc.). This study reveals that the efficiency of stabilizing heavy metals depends on the formation of stable mineral compounds containing heavy metals in pyrolysis biochar.

Keywords: co-pyrolysis, heavy metals, immobilization mechanism, sewage sludge

Procedia PDF Downloads 65

Authors: Yogita Patil-Sen

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Superparamagnetic Iron Oxide Nanoparticles (SPIONs) have become increasingly important materials for separation of specific bio-molecules, drug delivery vehicle, contrast agent for MRI and magnetic hyperthermia for cancer therapy. Hyperthermia is emerging as an alternative cancer treatment to the conventional radio- and chemo-therapy, which have harmful side effects. When subjected to an alternating magnetic field, the magnetic energy of SPIONs is converted into thermal energy due to movement of particles. The ability of SPIONs to generate heat and potentially kill cancerous cells, which are more susceptible than the normal cells to temperatures higher than 41 °C forms the basis of hyerpthermia treatement. The amount of heat generated depends upon the magnetic properties of SPIONs which in turn is affected by their properties such as size and shape. One of the main problems associated with SPIONs is particle aggregation which limits their employability in in vivo drug delivery applications and hyperthermia cancer treatments. Coating the iron oxide core with thermally responsive lipid based nanostructures tend to overcome the issue of aggregation as well as improve biocompatibility and can enhance drug loading efficiency. Herein we report suitability of SPIONs and silica coated core-shell SPIONs, which are further, coated with various lipids for drug delivery and magnetic hyperthermia applications. The synthesis of nanoparticles is carried out using the established methods reported in the literature with some modifications. The nanoparticles are characterised using Infrared spectroscopy (IR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Vibrating Sample Magnetometer (VSM). The heating ability of nanoparticles is tested under alternating magnetic field. The efficacy of the nanoparticles as drug carrier is also investigated. The loading of an anticancer drug, Doxorubicin at 18 °C is measured up to 48 hours using UV-visible spectrophotometer. The drug release profile is obtained under thermal incubation condition at 37 °C and compared with that under the influence of alternating magnetic field. The results suggest that the nanoparticles exhibit superparamagnetic behaviour, although coating reduces the magnetic properties of the particles. Both the uncoated and coated particles show good heating ability, again it is observed that coating decreases the heating behaviour of the particles. However, coated particles show higher drug loading efficiency than the uncoated particles and the drug release is much more controlled under the alternating magnetic field. Thus, the results demonstrate that lipid coated SPIONs exhibit potential as drug delivery vehicles for magnetic hyperthermia based cancer therapy.

Keywords: drug delivery, hyperthermia, lipids, superparamagnetic iron oxide nanoparticles (SPIONS)

Procedia PDF Downloads 231

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

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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: Y. Roumila, D. Meziani, R. Bagtache, K. Abdmeziem, M. Trari

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Heterogeneous photocatalysis over semiconductors has proved its effectiveness in the treatment of wastewaters since it works under soft conditions. It has emerged as a promising technique, giving rise to less toxic effluents and offering the opportunity of using sunlight as a sustainable and renewable source of energy. Many compounds have been used as photocatalysts. Though synthesized ones are intensively used, they remain expensive, and their synthesis involves special conditions. We thus thought of implementing a natural material, a phosphate ore, due to its low cost and great availability. Our work is devoted to the removal of hazardous organic pollutants, which cause several environmental problems and health risks. Among them, dye pollutants occupy a large place. This work relates to the study of the photodegradation of methyl violet (MV) and rhodamine B (RhB), in single and binary systems, under UV light and sunlight irradiation. Methyl violet is a triarylmethane dye, while RhB is a heteropolyaromatic dye belonging to the Xanthene family. In the first part of this work, the natural compound was characterized using several physicochemical and photo-electrochemical (PEC) techniques: X-Ray diffraction, chemical, and thermal analyses scanning electron microscopy, UV-Vis diffuse reflectance measurements, and FTIR spectroscopy. The electrochemical and photoelectrochemical studies were performed with a Voltalab PGZ 301 potentiostat/galvanostat at room temperature. The structure of the phosphate material was well characterized. The photo-electrochemical (PEC) properties are crucial for drawing the energy band diagram, in order to suggest the formation of radicals and the reactions involved in the dyes photo-oxidation mechanism. The PEC characterization of the natural phosphate was investigated in neutral solution (Na₂SO₄, 0.5 M). The study revealed the semiconducting behavior of the phosphate rock. Indeed, the thermal evolution of the electrical conductivity was well fitted by an exponential type law, and the electrical conductivity increases with raising the temperature. The Mott–Schottky plot and current-potential J(V) curves recorded in the dark and under illumination clearly indicate n-type behavior. From the results of photocatalysis, in single solutions, the changes in MV and RhB absorbance in the function of time show that practically all of the MV was removed after 240 mn irradiation. For RhB, the complete degradation was achieved after 330 mn. This is due to its complex and resistant structure. In binary systems, it is only after 120 mn that RhB begins to be slowly removed, while about 60% of MV is already degraded. Once nearly all of the content of MV in the solution has disappeared (after about 250 mn), the remaining RhB is degraded rapidly. This behaviour is different from that observed in single solutions where both dyes are degraded since the first minutes of irradiation.

Keywords: environment, organic pollutant, phosphate ore, photodegradation

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Authors: Dong Zhao

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Even though the recent claim of room temperature superconductivity by LK-99 was confirmed an unsuccessful attempt, this work reawakened people’s century striving to get applicable superconductors with Tc of room temperature or higher and under ambient pressure. One of the efforts was focusing on exploring the thorium salts. This is because certain thorium compounds revealed an unusual property of having both high electrical conductivity and diamagnetism or the so-called “coexistence of high electrical conductivity and diamagnetism.” It is well known that this property of the coexistence of high electrical conductivity and diamagnetism is held by superconductors because of the electron pairings. Consequently, the likelihood for these thorium compounds to have superconducting properties becomes great. However, as a surprise, these thorium salts possess this property at room temperature and atmosphere pressure. This gives rise to solid evidence for these thorium compounds to be room-temperature superconductors without a need for external pressure. Among these thorium compound superconductors claimed in that work, thorium di-iodide (ThI₂) is a unique one and has received comprehensive discussion. ThI₂ was synthesized and structurally analyzed by the single crystal diffraction method in the 1960s. Its special property of coexistence of high electrical conductivity and diamagnetism was revealed. Because of this unique property, a special molecular configuration was sketched. Except for an ordinary oxidation of +2 for the thorium cation, the thorium’s oxidation state in ThI₂ is +4. According to the experimental results, ThI₂‘s actual molecular configuration was determined as an unusual one of [Th4+(e-)2](I-)2. This means that the ThI₂ salt’s cation is composed of a [Th4+(e-)2]2+ cation core. In other words, the cation of ThI₂ is constructed by combining an oxidation state +4 of the thorium atom and a pair of electrons or an electron lone pair located on the thorium atom. This combination of the thorium atom and the electron lone pair leads to an oxidation state +2 for the [Th4+(e-)2]2+ cation core. This special construction of the thorium cation is very distinctive, which is believed to be the factor that grants ThI₂ the room temperature superconductivity. Actually, the key for ThI₂ to become a room-temperature superconductor is this characteristic electron lone pair residing on the thorium atom along with the formation of a network constructed by the thorium atoms. This network specializes in a way that allows the electron lone pairs to hop over it and, thus, to generate the supercurrent. This work will discuss, in detail, the special electrical and magnetic properties of ThI₂ as well as its structural features at ambient conditions. The exploration of how the electron pairing in combination with the structurally specialized network works together to bring ThI₂ into a superconducting state. From the experimental results, strong evidence has definitely pointed out that the ThI₂ should be a superconductor, at least at room temperature and under atmosphere pressure.

Keywords: co-existence of high electrical conductivity and diamagnetism, electron lone pair, room temperature superconductor, special molecular configuration of thorium di-iodide ThI₂

Procedia PDF Downloads 55

Authors: Soad Abubakr Abdelgalil, Gaber Attia Abo-Zaid, Mohamed Mohamed Yousri Kaddah

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Background: The Environmental Protection Agency has listed eggshell waste as the 15th most significant food industry pollution hazard. The utilization of eggshell waste as a source of renewable energy has been a hot topic in recent years. Therefore, finding a sustainable solution for the recycling and valorization of eggshell waste by investigating its potential to produce acid phosphatase (ACP) and organic acids by the newly-discovered B. sonorensis was the target of the current investigation. Results: The most potent ACP-producing B. sonorensis strain ACP2 was identified as a local bacterial strain obtained from the effluent of paper and pulp industries on basis of molecular and morphological characterization. The use of consecutive statistical experimental approaches of Plackett-Burman Design (PBD), and Orthogonal Central Composite Design (OCCD), followed by pH-uncontrolled cultivation conditions in a 7 L bench-top bioreactor, revealed an innovative medium formulation that substantially improved ACP production, reaching 216 U L⁻¹ with ACP yield coefficient Yp/x of 18.2 and a specific growth rate (µ) of 0.1 h⁻¹. The metals Ag+, Sn+, and Cr+ were the most efficiently released from eggshells during the solubilization process by B. sonorensis. The uncontrolled pH culture condition is the most suited and favored setting for improving the ACP and organic acids production simultaneously. Quantitative and qualitative analyses of produced organic acids were carried out using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Lactic acid, citric acid, and hydroxybenzoic acid isomer were the most common organic acids produced throughout the cultivation process. The findings of thermogravimetric analysis (TGA), differential scan calorimeter (DSC), scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), Fourier-Transform Infrared Spectroscopy (FTIR), and X-Ray Diffraction (XRD) analysis emphasize the significant influence of organic acids and ACP activity on the solubilization of eggshells particles. Conclusions: This study emphasized robust microbial engineering approaches for the large-scale production of a newly discovered acid phosphatase accompanied by organic acids production from B. sonorensis. The biovalorization of the eggshell waste and the production of cost-effective ACP and organic acids were integrated into the current study, and this was done through the implementation of a unique and innovative medium formulation design for eggshell waste management, as well as scaling up ACP production on a bench-top scale.

Keywords: chicken eggshells waste, bioremediation, statistical experimental design, batch fermentation

Procedia PDF Downloads 374

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

Procedia PDF Downloads 323

Authors: P. D. Pedrosa, J. M. A. Rebello, M. P. Cindra Fonseca

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Duplex stainless steels (DSS) exhibit a biphasic microstructure consisting of austenite and delta ferrite. Their high resistance to oxidation, and corrosion, even in H2S containing environments, allied to low cost when compared to conventional stainless steel, are some properties which make this material very attractive for several industrial applications. However, several of these industrial applications imposes cyclic loading to the equipments and in consequence fatigue damage needs to be a concern. A well-known way of improving the fatigue life of a component is by introducing compressive residual stress in its surface. Shot peening is an industrial working process which brings the material directly beneath component surface in a high mechanical compressive state, so inhibiting fatigue crack initiation. However, one must take into account the fact that the cyclic loading itself can reduce and even suppress these residual stresses, thus having undesirable consequences in the process of improving fatigue life by the introduction of compressive residual stresses. In the present work, shot peening was used to introduce residual stresses in several DSS samples. These were thereafter submitted to three different fatigue regimes: low, medium and high cycle fatigue. The evolution of the residual stress during loading were then examined on both surface and subsurface of the samples. It was used the DSS UNS S31803, with microstructure composed of 49% austenite and 51% ferrite. The treatment of shot peening was accomplished by the application of blasting in two Almen intensities of 0.25 and 0.39A. The residual stresses were measured by X-ray diffraction using the double exposure method and a portable equipment with CrK radiation and the (211) diffracting plane for the austenite phase and the (220) plane for the ferrite phase. It is known that residual stresses may arise when two regions of the same material experienced different degrees of plastic deformation. When these regions are separated in respect to each other on a scale that is large compared to the material's microstructure they are called macro stresses. In contrast, microstresses can largely vary over distances which are small comparable to the scale of the material's microstructure and must balance zero between the phases present. In the present work, special attention will be paid to the measurement of residual microstresses. Residual stress measurements were carried out in test pieces submitted to low, medium and high-cycle fatigue, in both longitudinal and transverse direction of the test pieces. It was found that after shot peening, the residual microstress is tensile in the austenite and compressive in the ferrite phases. It was hypothesized that the hardening behavior of the austenite after shot peening was probably due to its higher nitrogen content. Fatigue cycling can effectively change this stress state but this effect was found to be dependent of the shot peening intensity was well as the fatigue range.

Keywords: residual stresses, fatigue, duplex steel, shot peening

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Authors: Taro Komori, Toshiki Gushi, Akihito Anzai, Taku Hirose, Kaoru Toko, Shinji Isogami, Takashi Suemasu

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Ferrimagnetic antiperovskite Mn₄₋ₓNiₓN thin film exhibits both small saturation magnetization and rather large perpendicular magnetic anisotropy (PMA) when x is small. Both of them are suitable features for application to current induced domain wall motion devices using spin transfer torque (STT). In this work, we successfully grew antiperovskite 30-nm-thick Mn₄₋ₓNiₓN epitaxial thin films on MgO(001) and STO(001) substrates by MBE in order to investigate their crystalline qualities and magnetic and magneto-transport properties. Crystalline qualities were investigated by X-ray diffraction (XRD). The magnetic properties were measured by vibrating sample magnetometer (VSM) at room temperature. Anomalous Hall effect was measured by physical properties measurement system. Both measurements were performed at room temperature. Temperature dependence of magnetization was measured by VSM-Superconducting quantum interference device. XRD patterns indicate epitaxial growth of Mn₄₋ₓNiₓN thin films on both substrates, ones on STO(001) especially have higher c-axis orientation thanks to greater lattice matching. According to VSM measurement, PMA was observed in Mn₄₋ₓNiₓN on MgO(001) when x ≤ 0.25 and on STO(001) when x ≤ 0.5, and MS decreased drastically with x. For example, MS of Mn₃.₉Ni₀.₁N on STO(001) was 47.4 emu/cm³. From the anomalous Hall resistivity (ρAH) of Mn₄₋ₓNiₓN thin films on STO(001) with the magnetic field perpendicular to the plane, we found out Mr/MS was about 1 when x ≤ 0.25, which suggests large magnetic domains in samples and suitable features for DW motion device application. In contrast, such square curves were not observed for Mn₄₋ₓNiₓN on MgO(001), which we attribute to difference in lattice matching. Furthermore, it’s notable that although the sign of ρAH was negative when x = 0 and 0.1, it reversed positive when x = 0.25 and 0.5. The similar reversal occurred for temperature dependence of magnetization. The magnetization of Mn₄₋ₓNiₓN on STO(001) increases with decreasing temperature when x = 0 and 0.1, while it decreases when x = 0.25. We considered that these reversals were caused by magnetic compensation which occurred in Mn₄₋ₓNiₓN between x = 0.1 and 0.25. We expect Mn atoms of Mn₄₋ₓNiₓN crystal have larger magnetic moments than Ni atoms do. The temperature dependence stated above can be explained if we assume that Ni atoms preferentially occupy the corner sites, and their magnetic moments have different temperature dependence from Mn atoms at the face-centered sites. At the compensation point, Mn₄₋ₓNiₓN is expected to show very efficient STT and ultrafast DW motion with small current density. What’s more, if angular momentum compensation is found, the efficiency will be best optimized. In order to prove the magnetic compensation, X-ray magnetic circular dichroism will be performed. Energy dispersive X-ray spectrometry is a candidate method to analyze the accurate composition ratio of samples.

Keywords: compensation, ferrimagnetism, Mn₄N, PMA

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Authors: M. Kowalik, J. Masternak, K. Kazimierczuk, O. V. Khavryuchenko, B. Kupcewicz, B. Barszcz

Abstract:

Recently, the growing interest of chemists in metal-organic coordination polymers (MOCPs) is primarily derived from their intriguing structures and potential applications in catalysis, gas storage, molecular sensing, ion exchanges, nonlinear optics, luminescence, etc. Currently, we are devoting considerable effort to finding the proper method of synthesizing new coordination polymers containing S- or N-heteroaromatic carboxylates as linkers and characterizing the obtained Pb(II) compounds according to their structural diversity, luminescence, and thermal properties. The choice of Pb(II) as the central ion of MOCPs was motivated by several reasons mentioned in the literature: i) a large ionic radius allowing for a wide range of coordination numbers, ii) the stereoactivity of the 6s2 lone electron pair leading to a hemidirected or holodirected geometry, iii) a flexible coordination environment, and iv) the possibility to form secondary bonds and unusual non-covalent interactions, such as classic hydrogen bonds and π···π stacking interactions, as well as nonconventional hydrogen bonds and rarely reported tetrel bonds, Pb(lone pair)···π interactions, C–H···Pb agostic-type interactions or hydrogen bonds, and chelate ring stacking interactions. Moreover, the construction of coordination polymers requires the selection of proper ligands acting as linkers, because we are looking for materials exhibiting different network topologies and fluorescence properties, which point to potential applications. The reaction of Pb(NO₃)₂ with 1H-pyrrole-2-carboxylic acid (2prCOOH) leads to the formation of a new four-nuclear Pb(II) polymer, [Pb4(2prCOO)₈(H₂O)]ₙ, which has been characterized by CHN, FT-IR, TG, PL and single-crystal X-ray diffraction methods. In view of the primary Pb–O bonds, Pb1 and Pb2 show hemidirected pentagonal pyramidal geometries, while Pb2 and Pb4 display hemidirected octahedral geometries. The topology of the strongest Pb–O bonds was determined as the (4·8²) fes topology. Taking the secondary Pb–O bonds into account, the coordination number of Pb centres increased, Pb1 exhibited a hemidirected monocapped pentagonal pyramidal geometry, Pb2 and Pb4 exhibited a holodirected tricapped trigonal prismatic geometry, and Pb3 exhibited a holodirected bicapped trigonal prismatic geometry. Moreover, the Pb(II) lone pair stereoactivity was confirmed by DFT calculations. The 2D structure was expanded into 3D by the existence of non-covalent O/C–H···π and Pb···π interactions, which was confirmed by the Hirshfeld surface analysis. The above mentioned interactions improve the rigidity of the structure and facilitate the charge and energy transfer between metal centres, making the polymer a promising luminescent compound.

Keywords: coordination polymers, fluorescence properties, lead(II), lone electron pair stereoactivity, non-covalent interactions

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Authors: Chen Yuan, Nick Green, Stuart Blackburn

Abstract:

The investment casting process offers a great freedom of design combined with the economic advantage of near net shape manufacturing. It is widely used for the production of high value precision cast parts in particularly in the aerospace sector. Various combinations of materials have been used to produce the ceramic moulds, but most investment foundries use a silica based binder system in conjunction with fused silica, zircon, and alumino-silicate refractories as both filler and coarse stucco materials. However, in the context of advancing alloy technologies, silica based systems are struggling to keep pace, especially when net-shape casting titanium alloys. Study has shown that the casting of titanium based alloys presents considerable problems, including the extensive interactions between the metal and refractory, and the majority of metal-mould interaction is due to reduction of silica, present as binder and filler phases, by titanium in the molten state. Cleaner, more refractory systems are being devised to accommodate these changes. Although yttria has excellent chemical inertness to titanium alloy, it is not very practical in a production environment combining high material cost, short slurry life, and poor sintering properties. There needs to be a cost effective solution to these issues. With limited options for using pure oxides, in this work, a silica-free magnesia spinel MgAl₂O₄ was used as a primary coat filler and alumina as a binder material to produce facecoat in the investment casting mould. A comparison system was also studied with a fraction of the rare earth oxide Y₂O₃ adding into the filler to increase the inertness. The stability of the MgAl₂O₄/Al₂O₃ and MgAl₂O₄/Y₂O₃/Al₂O₃ slurries was assessed by tests, including pH, viscosity, zeta-potential and plate weight measurement, and mould properties such as friability were also measured. The interaction between the face coat and titanium alloy was studied by both a flash re-melting technique and a centrifugal investment casting method. The interaction products between metal and mould were characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDS). The depth of the oxygen hardened layer was evaluated by micro hardness measurement. Results reveal that introducing a fraction of Y₂O₃ into magnesia spinel can significantly increase the slurry life and reduce the thickness of hardened layer during centrifugal casting.

Keywords: titanium alloy, mould, MgAl₂O₄, Y₂O₃, interaction, investment casting

Procedia PDF Downloads 111

Authors: Smita Mondal, Dinesh Kumar Pandey, Prakash Biswas

Abstract:

During past two decades, considerable attention has been given to the value addition of biodiesel derived glycerol (~10wt.%) to make the biodiesel industry economically viable. Among the various glycerol value-addition methods, hydrogenolysis of glycerol to 1,2-propanediol is one of the attractive and promising routes. In this study, highly active and selective γ-Al₂O₃ supported bimetallic Cu-Ni catalyst was developed for selective hydrogenolysis of glycerol to 1,2-propanediol in the liquid phase. The catalytic performance was evaluated in a high-pressure autoclave reactor. The formation of mixed oxide indicated the strong interaction of Cu, Ni with the alumina support. Experimental results demonstrated that bimetallic copper-nickel catalyst was more active and selective to 1,2-PDO as compared to monometallic catalysts due to bifunctional behavior. To verify the effect of calcination temperature on the formation of Cu-Ni mixed oxide phase, the calcination temperature of 20wt.% Cu:Ni(1:1)/Al₂O₃ catalyst was varied from 300°C-550°C. The physicochemical properties of the catalysts were characterized by various techniques such as specific surface area (BET), X-ray diffraction study (XRD), temperature programmed reduction (TPR), and temperature programmed desorption (TPD). The BET surface area and pore volume of the catalysts were in the range of 71-78 m²g⁻¹, and 0.12-0.15 cm³g⁻¹, respectively. The peaks at the 2θ range of 43.3°-45.5° and 50.4°-52°, was corresponded to the copper-nickel mixed oxidephase [JCPDS: 78-1602]. The formation of mixed oxide indicated the strong interaction of Cu, Ni with the alumina support. The crystallite size decreased with increasing the calcination temperature up to 450°C. Further, the crystallite size was increased due to agglomeration. Smaller crystallite size of 16.5 nm was obtained for the catalyst calcined at 400°C. Total acidic sites of the catalysts were determined by NH₃-TPD, and the maximum total acidic of 0.609 mmol NH₃ gcat⁻¹ was obtained over the catalyst calcined at 400°C. TPR data suggested the maximum of 75% degree of reduction of catalyst calcined at 400°C among all others. Further, 20wt.%Cu:Ni(1:1)/γ-Al₂O₃ catalyst calcined at 400°C exhibited highest catalytic activity ( > 70%) and 1,2-PDO selectivity ( > 85%) at mild reaction condition due to highest acidity, highest degree of reduction, smallest crystallite size. Further, the modified Power law kinetic model was developed to understand the true kinetic behaviour of hydrogenolysis of glycerol over 20wt.%Cu:Ni(1:1)/γ-Al₂O₃ catalyst. Rate equations obtained from the model was solved by ode23 using MATLAB coupled with Genetic Algorithm. Results demonstrated that the model predicted data were very well fitted with the experimental data. The activation energy of the formation of 1,2-PDO was found to be 45 kJ mol⁻¹.

Keywords: glycerol, 1, 2-PDO, calcination, kinetic

Procedia PDF Downloads 142

Authors: Burçak Boztemur, Yue Xu, Laima Luo, M. Lütfi Öveçoğlu, Duygu Ağaoğulları

Abstract:

Tungsten (W) is used chiefly as plasma-facing material. However, it has some problems, such as brittleness after plasma exposure. High-entropy alloys (RHEAs) are a new opportunity for this deficiency. So, the neutron shielding behavior of WNbMoVTa and WNbMoVTaCr₀.₅Al compositions were examined against He⁺ irradiation in this study. The mechanical and irradiation properties of the WNbMoVTa base composition were investigated by adding the Al and Cr elements. The mechanical alloying (MA) for 6 hours was applied to obtain RHEA powders. According to the X-ray diffraction (XRD) method, the body-centered cubic (BCC) phase and NbTa phase with a small amount of WC impurity that comes from vials and balls were determined after 6 h MA. Also, RHEA powders were consolidated with the spark plasma sintering (SPS) method (1500 ºC, 30 MPa, and 10 min). After the SPS method, (Nb,Ta)C and W₂C₀.₈₅ phases were obtained with the decomposition of WC and stearic acid that is added during MA based on XRD results. Also, the BCC phase was obtained for both samples. While the Al₂O₃ phase with a small intensity was seen for the WNbMoVTaCr₀.₅Al sample, the Ta₂VO₆ phase was determined for the base sample. These phases were observed as three different regions according to scanning electron microscopy (SEM). All elements were distributed homogeneously on the white region by measuring an electron probe micro-analyzer (EPMA) coupled with a wavelength dispersive spectroscope (WDS). Also, the grey region of the WNbMoVTa sample was rich in Ta, V, and O elements. However, the amount of Al and O elements was higher for the grey region of the WNbMoVTaCr₀.₅Al sample. The high amount of Nb, Ta, and C elements were determined for both samples. Archimedes’ densities that were measured with alcohol media were closer to the theoretical densities of RHEAs. These values were important for the microhardness and irradiation resistance of compositions. While the Vickers microhardness value of the WNbMoVTa sample was measured as ~11 GPa, this value increased to nearly 13 GPa with the WNbMoVTaCr₀.₅Al sample. These values were compatible with the wear behavior. The wear volume loss was decreased to 0.16×10⁻⁴ from 1.25×10⁻⁴ mm³ by the addition of Al and Cr elements to the WNbMoVTa. The He⁺ irradiation was conducted on the samples to observe surface damage. After irradiation, the XRD patterns were shifted to the left because of defects and dislocations. He⁺ ions were infused under the surface, so they created the lattice expansion. The peak shifting of the WNbMoVTaCr₀.₅Al sample was less than the WNbMoVTa base sample, thanks to less impact. A small amount of fuzz was observed for the base sample. This structure was removed and transformed into a wavy structure with the addition of Cr and Al elements. Also, the deformation hardening was actualized after irradiation. A lower amount of hardening was obtained with the WNbMoVTaCr₀.₅Al sample based on the changing microhardness values. The surface deformation was decreased in the WNbMoVTaCr₀.₅Al sample.

Keywords: refractory high entropy alloy, microhardness, wear resistance, He⁺ irradiation

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