Search results for: powder x-ray diffraction

Authors: Houria Rezala, Jose Luis Valverde, Amaya Romero, Alessandra Molinari, Andrea Maldotti

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A pillared montmorillonite containing iron doped titania (Fe/Ti-PILC) has been prepared from a natural clay. This material has been characterized by X-ray diffraction, nitrogen adsorption, temperature programmed desorption of ammonia, inductively coupled plasma atomic emission spectroscopy, atomic absorption, and diffuse reflectance UV-VIS spectroscopy. The layer structure of Fe/Ti-PILC resulted to be ordered with an insertion of pillars, which caused a slight increase in the basal spacing of the clay. Its specific surface area was about three times larger than that of the parent Na-montmorillonite due principally to the creation of a remarkable microporous network. The doped material was a robust photocatalyst able to oxidize liquid alkyl aromatics to the corresponding carbonylic derivatives, using O2 as the oxidizing species, at mild pressure and temperature conditions. Accumulation of valuable carbonylic derivatives was possible since their over-oxidation to carbon dioxide was negligible. Fe/Ti-PILC was able to discriminate between toluene and cyclohexane in favor of the aromatic compound with an efficiency that is about three times higher than that of titanium pillared clays (Ti-PILC). It is likely that the addition of iron favored the formation of new acid sites able to interact with the aromatic substrate. Iron doping caused a significant TiO2 visible light-induced activity (wavelength > 400 nm) with only minor negative effects on its performance under UV-light irradiation (wavelength > 290 nm).

Keywords: alkyl aromatics oxidation, heterogeneous photocatalysis, iron doping, pillared clays

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Authors: Amit Keshav, Alok Sharma, Bidyut Mazumdar

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Colocasia esculenta leaves and roots are widely used in Asian countries, such as, India, Srilanka and Pakistan, as food and feed material. The root is high in carbohydrates and rich in zinc. The leaves and stalks are often traditionally preserved to be eaten in dry season. Leaf juice is stimulant, expectorant, astringent, appetizer, and otalgia. Looking at the medicinal uses of the plant leaves; phytochemicals were extracted from the plant leaves and were characterized using Fourier-transform infrared spectroscopy (FTIR) to find the functional groups. Phytochemical analysis of Colocasia esculenta (L.) leaf was studied using three solvents (methanol, chloroform, and ethanol) with soxhlet apparatus. Powder of the leaves was employed to obtain the extracts, which was qualitatively and quantitatively analyzed for phytochemical content using standard methods. Phytochemical constituents were abundant in the leave extract. Leaf was found to have various phytochemicals such as alkaloids, glycosides, flavonoids, terpenoids, saponins, oxalates and phenols etc., which could have lot of medicinal benefits such as reducing headache, treatment of congestive heart failure, prevent oxidative cell damage etc. These phytochemicals were identified using UV spectrophotometer and results were presented. In order to find the antioxidant activity of the extract, DPPH (2,2-diphenyl-1-picrylhydrazyl) method was employed using ascorbic acid as standard. DPPH scavenging activity of ascorbic acid was found to be 84%, whereas for ethanol it was observed to be 78.92%, for methanol: 76.46% and for chloroform: 72.46%. Looking at the high antioxidant activity, Colocasia esculenta may be recommended for medicinal applications. The characterizations of functional groups were analyzed using FTIR spectroscopy.

Keywords: antioxidant activity, Colocasia esculenta, leaves, characterization, FTIR

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Authors: B. Białecka, Z. Adamczyk, M. Cempa

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The use of ultrasounds in zeolization of fly ash can increase the efficiency of this process. The molar ratios of the reagents, as well as the time and temperature of the synthesis, are the main parameters determining the type and properties of the zeolite formed. The aim of the work was to create hydrosodalite in a short time (8h), with low NaOH concentration (3 M) and in low temperature (80°C). A zeolite material contained in fly ash from hard coal combustion in one of Polish Power Plant was subjected to hydrothermal alkaline synthesis. The phase composition of the ash consisted mainly of glass, mullite, quartz, and hematite. The dominant chemical components of the ash were SiO₂ (over 50%mas.) and Al₂O₃ (more than 28%mas.), whereas the contents of the remaining components, except Fe₂O₃ (6.34%mas.), did not exceed 4% mas. The hydrothermal synthesis of the zeolite material was carried out in the following conditions: 3M-solution of NaOH, synthesis time – 8 hours, 40 kHz-frequency ultrasounds during the first two hours of synthesis. The mineral components of the input ash as well as product after synthesis were identified in microscopic observations, in transmitted light, using X-ray diffraction (XRD) and electron scanning microscopy (SEM/EDS). The chemical composition of the input ash was identified by the method of X-ray fluorescence (XRF). The obtained material apart from phases found in the initial fly ash sample, also contained new phases, i.e., hydrosodalite and NaP-type zeolite. The chemical composition in micro areas of grains indicated their diversity: i) SiO₂ content was in the range 30-59%mas., ii) Al₂O₃ content was in the range 24-35%mas., iii) Na₂O content was in the range 6-15%mas. This clearly indicates that hydrosodalite forms hypertrophies with NaP type zeolite as well as relict grains of fly ash. A small amount of potassium in the examined grains is noteworthy, which may indicate the substitution of sodium with potassium. This is confirmed by the high value of the correlation coefficient between these two components.

Keywords: fly ash, hydrosodalite, ultrasounds, zeolite

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Authors: Bright Kwakye-Awuah, Elizabeth Von-Kiti, Isaac Nkrumah, Baah Sefa-Ntiri, Craig D. Williams

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Bauxite and kaolin from Ghana Bauxite Company mine site were used to synthesize zeolites. Bauxite served as the alumina source and kaolin the silica source. Synthesis variations include variation of aging time at constant crystallization time and variation of crystallization times at constant aging time. Characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDX) and Fourier transform infrared spectroscopy (FTIR) were employed in the characterization of the raw samples as well as the synthesized samples. The results obtained showed that the transformations that occurred and the phase of the resulting products were coordinated by the aging time, crystallization time, alkaline concentration and Si/Al ratio of the system. Zeolites A, X, Y, analcime, Sodalite, and ZK-14 were some of the phases achieved. Zeolite LTA was achieved with short crystallization times of 3, 5, 18 and 24 hours and a maximum aging of 24 hours. Zeolite LSX was synthesized with 24 hr aging followed with 24 hr hydrothermal treatment whilst zeolite Y crystallized after 48 hr of aging and 24 hr crystallization. Prolonged crystallization time produced a mixed phased product. Prolonged aging times, on the other hand, did not yield any zeolite as the sample was amorphous. Increasing the alkaline content of the reaction mixture above 5M introduced sodalite phase in the final product. The properties of the final products were comparable to zeolites synthesized from pure chemical reagents.

Keywords: bauxite, kaolin, aging, crystallization, zeolites

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Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: Tumelo W. P. Seadira, Thabang Ntho, Cornelius M. Masuku, Michael S. Scurrell

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A ternary Cu/TiO2/rGO photocatalysts was prepared using solvothermal method. Firstly, pure anatase TiO2 hollow spheres were prepared with titanium butoxide, ethanol, ammonium sulphate, and urea via hydrothermal method; and Cu nanoparticles were subsequently loaded on the surface of the hollow spheres by wet impregnation. During the solvothermal process, the deposition and well dispersion of Cu-TiO2 hollow spheres composites onto the graphene oxide surface, as well as the reduction of graphene oxide to graphene were achieved. The morphological and structural properties of the prepared samples were characterized by Brunauer-Emmett-Tellet (BET), X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscopy (TEM), and UV-vis DRS, and photoelectrochemical. The activities of the prepared catalysts were tested for hydrogen production via simultaneous photocatalytic water-splitting and glycerol reforming under visible light irradiation. The excellent photocatalytic activity of the Cu-TiO2-hollow-spheres/rGO catalyst was attributed the rGO which acts as both storage and transferor of electrons generated at the Cu and TiO2 heterojunction, thus increasing the electron-hole pairs separation. This paper reports the preparation of photocatalyst which is highly active by coupling reduced graphene oxide with nano-structured TiO2 with high surface area that can efficiently harvest the visible light for effective water-splitting and glycerol photocatalytic reforming in order to achieve efficient hydrogen evolution.

Keywords: glycerol reforming, hydrogen evolution, graphene oxide, Cu/TiO2-hollow-spheres/rGO

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Authors: Sanghamitra Acharya, Suwarna Datar

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Extensive use of digital and smart communication createsprolong expose of unwanted electromagnetic (EM) radiations. This harmful radiation creates not only malfunctioning of nearby electronic gadgets but also severely affects a human being. So, a suitable microwave absorbing material (MAM) becomes a necessary urge in the field of stealth and radar technology. Initially, Aluminum based hexa ferrite was prepared by sol-gel technique and for carbon derived composite was prepared by the simple one port chemical reduction method. Finally, composite films of Poly (Vinylidene) Fluoride (PVDF) are prepared by simple gel casting technique. Present work demands that aluminum-based hexaferrite phase conjugated with graphene in PVDF matrix becomes a suitable candidate both in commercially important X and Ku band. The structural and morphological nature was characterized by X-Ray diffraction (XRD), Field emission-scanning electron microscope (FESEM) and Raman spectra which conforms that 30-40 nm particles are well decorated over graphene sheet. Magnetic force microscopy (MFM) and conducting force microscopy (CFM) study further conforms the magnetic and conducting nature of composite. Finally, shielding effectiveness (SE) of the composite film was studied by using Vector network analyzer (VNA) both in X band and Ku band frequency range and found to be more than 30 dB and 40 dB, respectively. As prepared composite films are excellent microwave absorbers.

Keywords: carbon nanocomposite, microwave absorbing material, electromagnetic shielding, hexaferrite

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Authors: Tefera Worku Mekonnen, Hiseh Chih Tsai

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Enhancement of drug efficacy is essential in cancer treatment. The immune stimulator ovalbumin (Ova)-coated citric acid (AC-)-stabilized iron oxide nanoparticles (AC-IO-Ova NPs) and enhanced permeability and retention (EPR) based tumor targeted 4.5 (4.5G) poly(amidoamine) dendrimer-cisplatin nanocomplex (4.5GDP-Cis-pt NC) were used for enhanced anticancer efficiency. The formations of 4.5GDP-Cis-pt NC, AC-IO, and AC-IO-Ova NPs have been examined by FTIR, X-ray diffraction, Raman, and X-ray photoelectron spectroscopy. The conjugation of cisplatin (Cis-pt) with 4.5GDP was confirmed using carbon NMR. The tumor-specific 4.5GDP-Cis-pt NC provided ~45% and 28% cumulative cisplatin release in 72 h at pH 6.5 and 7.4, respectively. A significant immune response with high TNF-α and IL-6 cytokine secretion was confirmed when the co-incubation of AC-IO-Ova with RAW 264.7 or HaCaT cells. AC-IO-Ova NP was biocompatible in different cell lines, even at a high concentration (200 µg mL−1). In contrast, AC-IO-Ova NPs mixed with 4.5GDP-Cis-pt NC (Cis-pt at 15 µg mL−1) significantly increased the cytotoxicity against the cancer cells, which is dose-dependent on the concentration of AC-IO-Ova NPs. The increased anticancer effects may be attributed to the generation of reactive oxygen species (ROS). Moreover, the efficiency of anticancer cells may be further assisted by induction of an innate immune response via M1 macrophage polarization due to the presence of AC-IO-Ova NPs. We provide a better synergestic chemoimmunotherapeutic strategy to enhance the efficiency of anticancer of cisplatin via chemotherapeutic agent 4.5GDP-Cis-pt NC and induction of proinflammatory cytokines to stimulate innate immunity through AC-IO-Ova NPs against tumors.

Keywords: cisplatin-release, iron oxide, ovalbumin, poly(amidoamine) dendrimer

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Authors: Shefaa Mansour, Hassan Arafat, Shadi Hasan

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Management of reverse osmosis (RO) brine has become a major area of research due to the environmental concerns associated with it. This study worked on studying the feasibility of the direct contact membrane distillation (DCMD) system in the treatment of this RO brine. The system displayed great potential in terms of its flux and salt rejection, where different operating conditions such as the feed temperature, feed salinity, feed and permeate flow rates were varied. The highest flux of 16.7 LMH was reported with a salt rejection of 99.5%. Although the DCMD has displayed potential of enhanced water recovery from highly saline solutions, one of the major drawbacks associated with the operation is the fouling of the membranes which impairs the system performance. An operational run of 77 hours for the treatment of RO brine of 56,500 ppm salinity was performed in order to investigate the impact of fouling of the membrane on the overall operation of the system over long time operations. Over this time period, the flux was observed to have reduced by four times its initial flux. The fouled membrane was characterized through different techniques for the identification of the organic and inorganic foulants that have deposited on the membrane surface. The Infrared Spectroscopy method (IR) was used to identify the organic foulants where SEM images displayed the surface characteristics of the membrane. As for the inorganic foulants, they were identified using X-ray Diffraction (XRD), Ion Chromatography (IC) and Energy Dispersive Spectroscopy (EDS). The major foulants found on the surface of the membrane were inorganic salts such as sodium chloride and calcium sulfate.

Keywords: brine treatment, membrane distillation, fouling, characterization

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Authors: Bekan Bogale, Tsegaye Girma Asere, Tilahun Yai, Fekadu Melak

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Aims: To study photocatalytic degradation of methylene blue dye on cuprous oxide/graphene nanocomposite. Background: Cuprous oxide (Cu2O) nanoparticles are among the metal oxides that demonstrated photocatalytic activity. However, the stability of Cu2O nanoparticles due to the fast recombination rate of electron/hole pairs remains a significant challenge in their photocatalytic applications. This, in turn, leads to mismatching of the effective bandgap separation, tending to reduce the photocatalytic activity of the desired organic waste (MB). To overcome these limitations, graphene has been combined with cuprous oxides, resulting in cuprous oxide/graphene nanocomposite as a promising photocatalyst. Objective: In this study, Cu2O/graphene nanocomposite was synthesized and evaluated for its photocatalytic performance of methylene blue (MB) dye degradation. Method: Cu2O/graphene nanocomposites were synthesized from graphite powder and copper nitrate using the facile sol-gel method. Batch experiments have been conducted to assess the applications of the nanocomposites for MB degradation. Parameters such as contact time, catalyst dosage, and pH of the solution were optimized for maximum MB degradation. The prepared nanocomposites were characterized by using UV-Vis, FTIR, XRD, and SEM. The photocatalytic performance of Cu2O/graphene nanocomposites was compared against Cu2O nanoparticles for cationic MB dye degradation. Results: Cu2O/graphene nanocomposite exhibits higher photocatalytic activity for MB degradation (with a degradation efficiency of 94%) than pure Cu2O nanoparticles (67%). This has been accomplished after 180 min of irradiation under visible light. The kinetics of MB degradation by Cu2O/graphene composites can be demonstrated by the second-order kinetic model. The synthesized nanocomposite can be used for more than three cycles of photocatalytic MB degradation. Conclusion: This work indicated new insights into Cu2O/graphene nanocomposite as high-performance in photocatalysis to degrade MB, playing a great role in environmental protection in relation to MB dye.

Keywords: methylene blue, photocatalysis, cuprous oxide, graphene nanocomposite

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Authors: S. M. Giripunje, Shikha Jindal

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Zinc sulphide (ZnS) quantum dots (QDs) were synthesized successfully via simple sonochemical method. X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) analysis revealed the average size of QDs of the order of 3.7 nm. The band gap of the QDs was tuned to 5.2 eV by optimizing the synthesis parameters. UV-Vis absorption spectra of ZnS QD confirm the quantum confinement effect. Fourier transform infrared (FTIR) analysis confirmed the formation of single phase ZnS QDs. To fabricate the diode, blend of ZnS QDs and P3HT was prepared and the heterojunction of PEDOT:PSS and the blend was formed by spin coating on indium tin oxide (ITO) coated glass substrate. The diode behaviour of the heterojunction was analysed, wherein the ideality factor was found to be 2.53 with turn on voltage 0.75 V and the barrier height was found to be 1.429 eV. ZnS-Graphene QDs nanocomposite was characterised for the surface morphological study. It was found that the synthesized ZnS QDs appear as quasi spherical particles on the graphene sheets. The average particle size of ZnS-graphene nanocomposite QDs was found to be 8.4 nm. From voltage-current characteristics of ZnS-graphene nanocomposites, it is observed that the conductivity of the composite increases by 10⁴ times the conductivity of ZnS QDs. Thus the addition of graphene QDs in ZnS QDs enhances the mobility of the charge carriers in the composite material. Thus, the graphene QDs, with high specific area for a large interface, high mobility and tunable band gap, show a great potential as an electron-acceptors in photovoltaic devices.

Keywords: graphene, heterojunction, quantum confinement effect, quantum dots(QDs), zinc sulphide(ZnS)

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Authors: Ashirgul Kozhagulova, Ainash Shabdirova, Galym Tokazhanov, Minh Nguyen

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The synthetic rocks have been advantageous over the natural rocks in terms of availability and the consistent studying the impact of a particular parameter. The artificial rocks can be fabricated using variety of techniques such as mixing sand and Portland cement or gypsum, firing the mixture of sand and fine powder of borosilicate glass or by in-situ precipitation of calcite solution. In this study, sodium silicate solution has been used as the cementing agent for the quartz sand. The molded soft cylindrical sandstone samples are placed in the gas-tight pressure vessel, where the hardening of the material takes place as the chemical reaction between carbon dioxide and the silicate solution progresses. The vessel allows uniform disperse of carbon dioxide and control over the ambient gas pressure. Current paper shows how the bonding material is initially distributed in the intergranular space and the surface of the sand particles by the usage of Electron Microscopy and the Energy Dispersive Spectroscopy. During the study, the strength of the cement bond as a function of temperature is observed. The impact of cementing agent dosage on the micro and macro characteristics of the sandstone is investigated. The analysis of the cement bond at micro level helps to trace the changes to particles bonding damage after a potential yielding. Shearing behavior and compressional response have been examined resulting in the estimation of the shearing resistance and cohesion force of the sandstone. These are considered to be main input values to the mathematical prediction models of sand production from weak clastic oil reservoir formations.

Keywords: artificial sanstone, cement bond, microstructure, SEM, triaxial shearing

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Authors: Joon Y. Lee, Seung H. Shin, Ho H. Chun, Wan K. Jo

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Poly vinyl acetate (PVA)-based titania (TiO2)–carbon nanotube composite nanofibers (PVA-TCCNs) with various PVA-to-solvent ratios and PVA-based TiO2 composite nanofibers (PVA-TN) were synthesized using an electrospinning process, followed by thermal treatment. The photocatalytic activities of these nanofibers in the degradation of airborne monocyclic aromatics under visible-light irradiation were examined. This study focuses on the application of these photocatalysts to the degradation of the target compounds at sub-part-per-million indoor air concentrations. The characteristics of the photocatalysts were examined using scanning electron microscopy, X-ray diffraction, ultraviolet-visible spectroscopy, and Fourier-transform infrared spectroscopy. For all the target compounds, the PVA-TCCNs showed photocatalytic degradation efficiencies superior to those of the reference PVA-TN. Specifically, the average photocatalytic degradation efficiencies for benzene, toluene, ethyl benzene, and o-xylene (BTEX) obtained using the PVA-TCCNs with a PVA-to-solvent ratio of 0.3 (PVA-TCCN-0.3) were 11%, 59%, 89%, and 92%, respectively, whereas those observed using PVA-TNs were 5%, 9%, 28%, and 32%, respectively. PVA-TCCN-0.3 displayed the highest photocatalytic degradation efficiency for BTEX, suggesting the presence of an optimal PVA-to-solvent ratio for the synthesis of PVA-TCCNs. The average photocatalytic efficiencies for BTEX decreased from 11% to 4%, 59% to 18%, 89% to 37%, and 92% to 53%, respectively, when the flow rate was increased from 1.0 to 4.0 L min1. In addition, the average photocatalytic efficiencies for BTEX increased 11% to ~0%, 59% to 3%, 89% to 7%, and 92% to 13% , respectively, when the input concentration increased from 0.1 to 1.0 ppm. The prepared PVA-TCCNs were effective for the purification of airborne aromatics at indoor concentration levels, particularly when the operating conditions were optimized.

Keywords: mixing ratio, nanofiber, polymer, reference photocatalyst

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Authors: Afy Syahidan Achmad

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Tangkuban Perahu is located in West Java, Indonesia. It is active stratovolcano type and still showing hidrothermal activity. The main purpose of this study is to find correlation between subsurface structure and hidrothermal activity on the surface. Using topographic map, SRTM images, and field observation, geological condition and alteration area was mapped. Alteration sample analyzed trough petrographic analysis and X-Ray Diffraction (XRD) analysis. Altered rock in study area showing white-yellowish white colour, and texture changing variation from softening to hardening because of alteration by sillica and sulphur. Alteration mineral which can be observed in petrographic analysis and XRD analysis consist of crystobalite, anatase, alunite, and pyrite. This mineral assemblage showing advanced argillic alteration type with West-East alteration area orientation. Alteration area have correlation with manifestation occurance such as steam vents, solfatara, and warm to hot pools. Most of manifestation occured in main crater like Ratu Crater and Upas crater, and parasitic crater like Domas Crater and Jarian Crater. This manifestation indicates permeability in subsurface which can be created trough structural process with same orientation. For further study geophysics method such as Magneto Telluric (MT) and resistivity can be required to find permeability zone pattern in Tangkuban Perahu subsurface.

Keywords: alteration, advanced argillic, Tangkuban Perahu, XRD, crystobalite, anatase, alunite, pyrite

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Authors: Abrar Hussain, Kuen-Song Lin, Sayed Maeen Badshah, Jamshid Hussain

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The conversion of CO₂ into versatile, useful compounds such as fuels and other chemicals remains a challenging frontier in research, demanding the innovation of increasingly effective catalysts. In the present work, a catalyst-incorporating zirconium (Zr) modification within CuO–ZnO–Al₂O₃ (CZA) was synthesized via a co-precipitation method to convert CO₂ into methanol. Furthermore, bio-HZSM-5 was used to promote methanol dehydration to produce dimethyl ether (DME). We prepared the porous hierarchy bio-HZSM-5 with remarkable pore connectivity by utilizing an economical loofah sponge and rice husks as biotemplates. The synthesized catalysts were characterized using Field Emission Scanning Electron Microscopy (FE-SEM), X–ray diffraction (XRD), N₂ adsorption (BET), temperature-programmed desorption (NH₃-TPD) and thermogravimetric analysis (TGA). The Zr addition improved the performance of the CZZA catalyst as a structural promoter, leading to increased DME selectivity and total carbon conversion by enhancing active sites, surface area, and the synergistic interfaces between CuO and ZnO. The presence of silicon in the biomass, notably from the loofah sponge (0.016 wt %) and rice husks (8.3 wt %), also performed a pivotal role in the preparation of bio-HZSM-5. Furthermore, contrasted to the CZZA/com-ZSM-5 catalyst, the integration of CZZA with bio-HZSM-5-L bifunctional catalyst achieved the highest DME yield (12.1 %), DME selectivity (58.6%), CO₂ conversion (22.5%) at 280 °C and 30 bar. The payback time for 5 and 10-tons per day (5 and10-TPD) DME formation using the catalytic process of CO₂ from petrochemical refinery plant waste gas emissions was 2.98 and 2.44 years, respectively.

Keywords: Cost assessment, Dimethyl ether, low-cost bio-HZSM-5, CZZA catalyst, CO₂ hydrogenation

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Authors: Ekramul Hoque, Zinat Ara Eakut Zarin, Ershad Ali

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The growth and development of explants is governed by the effect of nutrient medium. Ammonium nitrate (NH4NO3) as a major salt of stock solution-1 for the preparation of tissue culture medium. But, it has several demerits on human civilization. It is use for the preparation of bomb and other destructive activities. Hence, it is totally ban in our country. A new chemical was identified as a substitute of ammonium nitrate. The concentrations of the other ingredients of major and minor salt were modified from the MS medium. The formulation of new medium is totally different from the MS nutrient composition. The most widely use MS medium composition was used as first check treatment and MS powder (Duchefa Biocheme, The Netherland) was used as second check treatment. The experiments were carried out at the Department of Biotechnology, Sher-e-Bangla Agricultural University, Dhaka, Bangladesh. Two potato varieties viz. Diamant and Asterix were used as experimental materials. The regeneration potentiality of potato onto new medium was best as compare with the two check treatments. The traits -node number, leaf number, shoot length, root lengths were highest in new medium. The plantlets were healthy, robust and strong as compare to plantlets regenerated from check treatments. Three subsequent sub-cultures were made in the new medium to observe the growth pattern of plantlet. It was also showed the best performance in all the parameter under studied. The regenerated plantlet produced good quality minituber under field condition. Hence, it is concluded that, a new plant tissue culture medium as discovered from the Department of Biotechnology, Sher-e-Bangla Agricultural University, Dhaka, Bangladesh under the leadership of Professor Dr. Md. Ekramul Hoque.

Keywords: new medium, potato, regeneration, ammonium nitrate

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Authors: Rania Hanafi Said, Rasha Mohamed Taha

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Background: By using nanoparticles as drug delivery, it may be possible to avoid the drawbacks of systemic antibiotic dosing, including bacterial antibiotic resistance. The goal of this study was to see how well tetracycline loaded on nanochitosan worked to treat gingival inflammation in albino rats caused by Porphyromonas gingivalis. The study analyzed immunohistochemically the localization of the pro-inflammatory cytokine Interleukin-1beta (IL-1β). Material and methods: In this study, fifty mature male albino rats weighing 150 to 180 grams each were used. They were randomly divided into five groups. We checked for weight changes in rats. Ten male albino rats were included in Group I, which served as a negative control group. Ten rats were included in Group II, where they were exposed once to Porphyromonas. Group III contained ten rats, which were treated the same as Group II plus daily injections of diluted tetracycline powder at the infection sites. Ten rats in Group IV received the same procedure as those in Group II before receiving daily injections of nanochitosan at the injection sites. Finally, Group V, which had ten rats. Following the same protocol as Group II, they received localized injections of tetracycline loaded on nanochitosan once daily. Rats' gingivae were extracted and prepared after they were anesthetized. The biopsies were examined histologically and immunohistochemically by light microscopy. Results: Groups I and V had a nearly normal histological appearance of gingival tissue. In Groups II, III, and IV, degeneration was seen because the epithelial cells were bigger, collagen fibers were pulling away from the lamina propria connective tissue, and the basement membranes had come to an end. There was no discernible difference between groups V and I when they were examined immunohistochemically. Conclusion: The use of nano chitosan as a tetracycline carrier is a novel technique to overcome the drug's rising level of resistance.

Keywords: Immunohistochemistry, Nanochitosan, porphyromonas gingivitis, Tetracycline

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Authors: Bryce R. Jolley, Michael Uchic

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This study presents initial results toward the correlative characterization of inherent defects of Ti-6Al-4V additive manufacture (AM). X-Ray Computed Tomography (CT) defect data are compared and correlated with microscopic photographs obtained via automated serial sectioning. The metal AM specimen was manufactured out of Ti-6Al-4V virgin powder to specified dimensions. A post-contour was applied during the fabrication process with a speed of 1050 mm/s, power of 260 W, and a width of 140 µm. The specimen was stress relief heat-treated at 16°F for 3 hours. Microfocus CT imaging was accomplished on the specimen within a predetermined region of the build. Microfocus CT imaging was conducted with parameters optimized for Ti-6Al-4V additive manufacture. After CT imaging, a modified RoboMet. 3D version 2 was employed for serial sectioning and optical microscopy characterization of the same predetermined region. Automated montage capture with sub-micron resolution, bright-field reflection, 12-bit monochrome optical images were performed in an automated fashion. These optical images were post-processed to produce 2D and 3D data sets. This processing included thresholding and segmentation to improve visualization of defect features. The defects observed from optical imaging were compared and correlated with the defects observed from CT imaging over the same predetermined region of the specimen. Quantitative results of area fraction and equivalent pore diameters obtained via each method are presented for this correlation. It is shown that Microfocus CT imaging does not capture all inherent defects within this Ti-6Al-4V AM sample. Best practices for this correlative effort are also presented as well as the future direction of research resultant from this current study.

Keywords: additive manufacture, automated serial sectioning, computed tomography, nondestructive evaluation

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Authors: S. Nqayi, B. Sondezi

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A rare-earth-based Sm₂MnRuO₆₊δ (SMRO) double perovskite was prepared using a high-temperature solid-state reaction. The structural, morphological, chemical, thermodynamic, and magnetic properties were measured with X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), X-ray photoemission spectroscopy (XPS), and vibrating sample magnetometer (VSM), respectively. The XRD revealed a tetragonal structure belonging to the I4/mmm space group, number 139, with linear Mn−O−Ru bonds. Replacing the well-studied alkaline earth metal with a rare-earth element increased the Mn-O bond length difference between the shorter equatorial (Mn-Oab) and the axial (Mn-Oc) bonds by approximately 6.3%. The elemental composition showed an O-rich double perovskite with a Ru deficit, which encourages the formation of a Ru⁶⁺ (d²) state. XPS spectra of Sm-3d, Ru-3d, and Mn-2p revealed the coexistence of a double oxidation state for each cation; Sm²⁺, Sm³⁺, Ru³⁺, Ru⁶⁺, Mn²⁺ , and Mn³⁺, in varying proportions. Entropy studies showed drastic ordering of spins at low temperatures (up to 12.4 K), whilst increasing temperatures above this point resulted in a drastic increase of disorder of the spins (up to 43.26 K), beyond which a constant slope of entropy is observed. Magnetic measurements revealed two magnetic ground states at TN = 12.4 K and TC = 43.3 K ordering antiferromagnetically (AFM) and ferromagnetically (FM), respectively. Kneller fit further showed that the materials become completely paramagnetic at TB = 88.1 K, (the blocking temperature). The existence of ferromagnetic (FM) super-exchange coupling in this work originating from Mn³⁺ (t³₂𝓰e¹𝓰)−O−Ru³⁺ (t⁵₂𝓰e⁰𝓰) and Mn²⁺ (t³₂𝓰e²𝓰−O−Ru⁶⁺ (t²₂𝓰e⁰𝓰) which plays an important role in suppressing the Mn/Ru−O−Mn/Ru antiferromagnetic (AFM) interactions.

Keywords: solid-state reaction, super-exchange coupling, ferromagnetic, Kneller’s law, entropy

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Authors: Mohamed M. A. Rahoma

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A better understanding of the factors that control the resistivity values of Sandstone reservoirs is very important for petroleum exploration and production. This study is an attempt to find out the factors that could be the reason for the decrease in resistivity values of the Lower Akakus Sandstones, which are the main reservoir in the area in an onshore field located in the northern part of Ghadames Basin - Northwest of Libya in the contracted area 47, block 2 The study achieved is based on: 30 core chip samples taken from two wells (A3-47/02 and J1-47/02) and Routine Core Analysis (RCA). The results of petrography analysis (thin section, X-ray diffraction and SEM) demonstrated that the depth sits (intervals) which illustrated low resistivity values have a relatively high content of diagenetic clay and cement minerals, hence we can conclude that diagenetic events have a more significant impact on the resistivity values of studied interval for possibly two following reasons: The first essential reason, the extensive micro pores that mostly exist within clay minerals (Chlorite and Kaolinite where, about 30-50 % of their composition considered micro pores), resistivity log read low as noticed through the study. The highest value of micro pores recorded in core1 of J1-47/02 well due to most likely the kaolinite amount which was a slightly higher than the chlorite amount in this well (the bond water porosity for chlorite clay considered relatively the lowest porosity compared to other clay minerals). The second reason, the presence of diagenetic cement minerals (Siderite and Hematite, which contain an iron element as one of their components) within the studied interval as remarked from my study may cause decreasing in resistivity of the formation of the reservoir.

Keywords: diagenetic cement, diagenetic clay, resistivity, petrography analysis

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Authors: Yahia Massinissa, Benhouda Afaf, Benbia Souhila, Meddour Noura, Takellalet Karima, Zeroual Amina

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Introduction: chenopodiaceae family species are known for their important biological activity, in which Atriplex halimus belongs . However, the inflammatory effect of this plant leaves has not been studied. This work aimed at assessing the anti- inflammatory and hemostatic activities of the methanolic extract AHMeOH of Atriplex halimus’s leaves. Methods: The extract was obtained using sonication of leaves powder in 80 % methanol. The analysis of phenolic compounds was carried out using thin-layer chromatography (TLC).The anti-inflammatory activity was determined by studying the plasmical membrane stabilization and albumin denaturation inhibition, the hemostatic activity was evaluated by measuring the plasma in the blood. Results: Quantitative determination of total flavonoids reveals that AHMeOH is rich in flavonoids (16 ± 0.88 μg Q / mg extract) and polyphenols (20 ± 0.20 μg AG / mg extract). about anti-inflammatory activity, the tests show that AHMeOH has a significant effect (P≤0.05) of inhibiting hypotonic-induced hemolysis with concentrations (100 and 200 μg / ml) with 77.55 and 90% respectively, and heat-induced hemolysis with percentages 81.75% and 87.44% respectively with significant difference (P ≤0.05). The obtained results with this plant reveal that the inhibition of denaturation of albumin is dose dependent. The concentration of 400 μg / ml gives denaturation inhibition of 81.00 ± 17.70% and the concentration 600 μg / ml gives an effect of 82.95 ± 17.40%. Regarding the haemostatic activity our extract with the doses 10 mg / ml, 20 mg / ml and 30 mg / ml confer a decrease of the plasma recalcification time in the tube, these concentrations could prolong the time of coagulation significantly compared to the control (P≤0.001). This result is an interesting indication in favor of haemostatic activity of AHMeOH. Conclusion: Atriplex Halimus has a strong anti-inflammatory activity and constitutes a potential source for the development of new treatments.

Keywords: albumin, atriplex halimus, hemostatic activity, methanolic extract

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Authors: Mahmoud A Rabah, Sabah M. Abelbasir

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Lead-calcium alloy containing up to 0.10% calcium was recovered from spent rechargeable sealed acid lead batteries. Two techniques were investigated to explore the effect of flux salts on the extent and quality of the recovered alloy, pyro-metallurgical and electrochemical methods. About 10 kg of the spent batteries were collected for testing. The sample was washed with hot water and dried. The plastic cases of the batteries were mechanically cut, and the contents were dismantled manually, the plastic containers were shredded for recycling. The electrode plates were freed from the loose powder and placed in SiC crucible and covered with alkali chloride salts. The loaded crucible was heated in an electronically controlled chamber furnace type Nabertherm C3 at temperatures up to 800 °C. The obtained metals were analyzed. The effect of temperature, rate of heating, atmospheric conditions, composition of the flux salts on the extent and quality of the recovered products were studied. Results revealed that the spent rechargeable batteries contain 6 blocks of 6 plates of Pb-Ca alloy each. Direct heating of these plates in a silicon carbide crucible under ambient conditions produces lead metal poor in calcium content ( < 0.07%) due to partial oxidation of the alloying calcium element. Rate of temperature increase has a considerable effect on the yield of the lead alloy extraction. Flux salts composition benefits the recovery process. Sodium salts are more powerful as compared to potassium salts. Lead calcium alloy meeting the standard specification was successfully recovered from the spent rechargeable acid lead batteries with a very competitive cost to the same alloy prepared from primary resources.

Keywords: rechargeable lead batteries, lead-calcium alloy, waste recovery, flux salts, thermal recovery

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Authors: Ibetombi Soibam

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Li-Zn-Ni ferrite having the compositional formula Li0.4-0.5xZn0.2NixFe2.4-0.5xO4 where x = 0.02 ≤ x ≤0.1 in steps of 0.02 was fabricated by the citrate precursor method. In this method, metal nitrates and citric acid was used to prepare the gel which exhibit self-propagating combustion behavior giving the required ferrite sample. The ferrite sample was given a pre-firing at 650°C in a programmable conventional furnace for 3 hours with a heating rate of 5°C/min. A series of the sample was finally given conventional sintering (CS) at 1040°C after the pre-firing process. Another series was given microwave sintering (MS) at 1040°C in a programmable microwave furnace which uses a single magnetron operating at 2.45 GHz frequency. X- ray diffraction pattern confirmed the spinel phase structure for both the series. The theoretical and experimental density was calculated. It was observed that densification increases with the increase in Ni concentration in both the series. However, samples sintered by microwave technique was found to be denser. The microstructure of the two series of the sample was examined using scanning electron microscopy (SEM). Dielectric properties have been investigated as a function of frequency and composition for both series of samples sintered by CS and MS technique. The variation of dielectric constant with frequency show dispersion for both the series. It was explained in terms of Koop’s two layer model. From the analysis of dielectric measurement, it was observed that the value of room temperature dielectric constant decreases with the increase in Ni concentration for both the series. The microwave sintered samples show a lower dielectric constant making microwave sintering suitable for high-frequency applications. The possible mechanisms contributing to all the above behavior is being discussed.

Keywords: citrate precursor, dielectric constant, ferrites, microwave sintering

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Authors: Isam A. H. Al Zubaidy

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A quick process may be needed to get the benefit the big generated quantity of waste oil sludge (WOS). The process includes the mixing process of WOS with commercial diesel fuel. Different ratios of WOS to diesel fuel were prepared ranging 1:1 to 20:1 by mass. The mixture was continuously mixing for 10 minutes using bench type overhead stirrer and followed by filtration process to separate the soil waste from filtrate oil product. The quantity and the physical properties of the oil filtrate were measured. It was found that the addition of up to 15% WOS to diesel fuel was accepted without dramatic changes to the properties of diesel fuel. The amount of waste oil sludge was decreased by about 60% by mass. This means that about 60 % of the mass of sludge was recovered as light fuel oil. The physical properties of the resulting fuel from 10% sludge mixing ratio showed that the specific gravity, ash content, carbon residue, asphaltene content, viscosity, diesel index, cetane number, and calorific value were affected slightly. The color was changed to light black color. The sulfur content was increased also. This requires other processes to reduce the sulfur content of the resulting light fuel. A new desulfurization process was achieved using adsorption techniques with activated biomaterial to reduce the sulfur content to acceptable limits. Adsorption process by ZnCl₂ activated date palm kernel powder was effective for improvement of the physical properties of diesel like fuel. The final sulfur content was increased to 0.185 wt%. This diesel like fuel can be used in all tractors, buses, tracks inside and outside the refineries. The solid remaining seems to be smooth and can be mixed with asphalt mixture for asphalting the roads or can be used with other materials as an asphalt coating material for constructed buildings. Through this process, valuable fuel has been recovered, and the amount of waste material had decreased.

Keywords: oil sludge, diesel fuel, blending process, filtration process

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Authors: Shuangxin Wu

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Superalloy ultra-thin-walled components occupy a considerable proportion of aero engines and play an increasingly important role in structural weight reduction and performance improvement. To solve problems such as high deformation resistance and poor formability at room temperature, the introduction of pulse current in the processing process can improve the plasticity of metal materials, but the influence mechanism of pulse current on the forming limit of superalloy ultra-thin sheet is not clear, which is of great significance for determining the material processing window and improving the micro-forming process. The effect of pulse current on the microstructure evolution of superalloy thin plates was observed by optical microscopy (OM) and X-ray diffraction topography (XRT) by applying pulse current to GH3039 with a thickness of 0.2mm under plane strain and uniaxial tensile states. Compared with the specimen without pulse current applied at the same temperature, the internal void volume fraction is significantly reduced, reflecting the non-thermal effect of pulse current on the growth of micro-pores. ED (electrically deforming) specimens have larger and deeper dimples, but the elongation is not significantly improved because the pulse current promotes the void coalescence process, resulting in material fracture. The electro-plastic phenomenon is more obvious in the plane strain state, which is closely related to the effect of stress triaxial degree on the void evolution under pulsed current.

Keywords: pulse current, superalloy, ductile fracture, void damage

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Authors: Emrah Yaliniz, Ali Kalkanli

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ZE41A magnesium alloy has been extensively used in aerospace industry, especially for use in rotorcraft transmission casings. Due to the improved mechanical properties, the latest generation of magnesium casting alloy EV31A-T6 (Elektron 21® specified in AMS 4429) is seen as a potential replacement for ZE41A in terms of strength. Therefore, the necessity of enhancement has been arisen for ZE41A in order to avoid fully replacement. The main element affecting the strength of ZE41A is Zirconium (Zr), which acts as a grain refiner. The specified range of Zr element for ZE41A alloy is between 0.4 wt % and 1.0 wt % (unless otherwise stated by weight percentage after this point) as stated in AMS 4439. This paper investigates the effects of Zr amount on tensile and metallurgical properties of ZE41A magnesium alloy. The Zr alloying amount for the research has been chosen as 0.5 % and 1 %, which are standard amounts in a commercial alloy (average of 0.4-0.6%) and maximum percent in the standard, separately. 1 % Zr amount has been achieved via Zirmax (66.7 Mg-33.3 Zr) master alloy addition. The ultimate tensile strength of ZE41A with 1% Zr has been increased up to about 220-225 MPa in comparison to 200 MPa given in AMS 4439. The reason for the increase in strength with the addition of Zirmax is based on the decrease in grain size, which was measured about 30 µm. Optical microscope, scanning electron microscopy (SEM) and X-ray Diffraction (XRD) were used to detect the change in the microstructural futures via alloying. The zirconium rich coring at the center of the grains was observed in addition to the grain boundary intermetallic phases and bulk Mg-rich matrix. The solidification characteristics were also identified by using the cooling curve obtained from the sand casting mold during cooling of the alloys.

Keywords: aerospace, grain refinement, magnesium, sand casting, ZE41A

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Authors: Jefri Draup, Antoine Ambard, Chi-Toan Nguyen

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Zirconium alloys exhibit solid-state phase transformations under thermal loading. These can lead to a significant evolution of the microstructure and associated mechanical properties of materials used in nuclear fuel cladding structures. Therefore, the ability to capture effects of phase transformation on the material constitutive behavior is of interest during conditions of severe transient thermal loading. Whilst typical Avrami, or Johnson-Mehl-Avrami-Kolmogorov (JMAK), type models for phase transformations have been shown to have a good correlation with the behavior of Zircaloy-4 under constant heating rates, the effects of variable and fast heating rates are not fully explored. The present study utilises the results of in-situ high energy synchrotron X-ray diffraction (SXRD) measurements in order to validate the phase transformation models for Zircaloy-4 under fast variable heating rates. These models are used to assess the performance of fuel cladding structures under loss of coolant accident (LOCA) scenarios. The results indicate that simple Avrami type models can provide a reasonable indication of the phase distribution in experimental test specimens under variable fast thermal loading. However, the accuracy of these models deteriorates under the faster heating regimes, i.e., 100Cs⁻¹. The studies highlight areas for improvement of simple Avrami type models, such as the inclusion of temperature rate dependence of the JMAK n-exponent.

Keywords: accident, fuel, modelling, zirconium

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Authors: Askar Kilmametov, Julia Ivanisenko, Boris Straumal, Horst Hahn

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The high-pressure α- to ω-phase transition was discovered in elemental Ti and Zr fifty years ago using static high pressure and then observed to appear between 2 and 12 GPa at room temperature, depending on the experimental technique, the pressure environment, and the sample purity. The fact that ω-phase is retained in a metastable state in ambient condition after the removal of the pressure has been used to check the changes in magnetic and superconductive behavior, electron band structure and mechanical properties. However, the fundamental knowledge on a combination of both mechanical treatment and high applied pressure treatments for ω-phase formation in Ti alloys is currently lacking and has to be studied in relation to improved mechanical properties of bulk nanostructured states. In the present study, nanostructured (α+β) Ti alloys containing β-stabilizing elements such as Co, Fe, Cr, Nb were performed by severe plastic deformation, namely high pressure torsion (HPT) technique. HPT-induced α- to ω-phase transformation was revealed in dependence on applied pressure and shear strains by means of X-ray diffraction, transmission electron microscopy, and differential scanning calorimetry. The transformation kinetics was compared with the kinetics of pressure-induced transition. Orientation relationship between α-, β- and ω-phases was taken into consideration and analyzed according to theoretical calculation proposed earlier. The influence of initial state before HPT appeared to be considerable for subsequent α- to ω-phase transition. Thermal stability of the HPT-induced ω-phase was discussed as well in the frame of mechanical behavior of Ti and Ti-based alloys produced by shear deformation under high applied pressure.

Keywords: bulk nanostructured materials, high pressure phase transitions, severe plastic deformation, titanium alloys

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Authors: Z. Kassab, A. Aboulkas, A. Barakat, M. El Achaby

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The red algae are available enormously around the world and their exploitation for the production of agar product has become as an important industry in recent years. However, this industrial processing of red algae generated a large quantity of solid fibrous wastes, which constitute a source of a serious environmental problem. For this reason, the exploitation of this solid waste would help to i) produce new value-added materials and ii) to improve waste disposal from environment. In fact, this solid waste can be fully utilized for the production of cellulose microfibers and nanocrystals because it consists of large amount of cellulose component. For this purpose, the red algae waste was chemically treated via alkali, bleaching and acid hydrolysis treatments with controlled conditions, in order to obtain pure cellulose microfibers and cellulose nanocrystals. The raw product and the as-extracted cellulosic materials were successively characterized using serval analysis techniques, including elemental analysis, X-ray diffraction, thermogravimetric analysis, infrared spectroscopy and transmission electron microscopy. As an application, the as extracted cellulose nanocrystals were used as nanofillers for the production of polymer-based composite films with improved thermal and tensile properties. In these composite materials, the adhesion properties and the large number of functional groups that are presented in the CNC’s surface and the macromolecular chains of the polymer matrix are exploited to improve the interfacial interactions between the both phases, improving the final properties. Consequently, the high performances of these composite materials can be expected to have potential in packaging material applications.

Keywords: cellulose nanowhiskers, food packaging, polymer composites, red algae waste

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Authors: Tiziana Biasutti, Daniela Rigamonti, Lorenzo Palmiotti, Adelaide Nespoli, Paolo Bettini

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Aerospace industry is based on the continuous development of new technologies and solutions that allows constant improvement of the systems. Shape Memory Alloys are smart materials that can be used as dampers due to their pseudoelastic effect. The purpose of the research was to design a passive damper in Nitinol, manufactured by Selective Laser Melting, for space applications to reduce vibration between different structural parts in space structures. The powder is NiTi (50.2 at.% of Ni). The structure manufactured by additive technology allows us to eliminate the presence of joint and moving parts and to have a compact solution with high structural strength. The designed dampers had single or double cell structures with three different internal angles (30°, 45° and 60°). This particular shape has damping properties also without the pseudoelastic effect. For this reason, the geometries were reproduced in different materials, SS316L and Ti6Al4V, to test the geometry loss factor. The mechanical performances of these specimens were compared to the ones of NiTi structures, pointing out good damping properties of the designed structure and the highest performances of the NiTi pseudoelastic effect. The NiTi damper was mechanically characterized by static and dynamic tests and with DSC and microscope observations. The experimental results were verified with numerical models and with some scaled steel specimens in which optical fibers were embedded. The realized structure presented good mechanical and damping properties. It was observed that the loss factor and the dissipated energy increased with the angles of the cells.

Keywords: additive manufacturing, damper, nitinol, pseudo elastic effect, selective laser melting, shape memory alloys

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