Search results for: powder X-ray diffraction

Authors: Princess Stephanie P. Llanos, Rinlee Butch M. Cervera

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Lithium iron phosphate (LiFePO4) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, carbon-coated nanograined LiFePO4 is synthesized via wet chemistry method at a low temperature of 400 °C and investigated its performance as a cathode in Lithium battery. The X-ray diffraction pattern of the synthesized samples can be indexed to an orthorhombic LiFePO4 structure. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LiFePO4 and coating of amorphous carbon layer. Elemental mapping using Energy dispersive spectroscopy analysis revealed the homogeneous dispersion of Fe, P, O, and C elements. On the other hand, the electrochemical performances of the synthesized cathodes were investigated using cyclic voltammetry, galvanostatic charge/discharge tests with different C-rates, and cycling performances. Galvanostatic charge and discharge measurements revealed that the sample sintered at 400 °C for 3 hours with carbon coating demonstrated the highest capacity among the samples which reaches up to 160 mAhg⁻¹ at 0.1C rate.

Keywords: cathode, charge-discharge, electrochemical, lithium batteries

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Authors: Yung-Jin Weng, Chia-Chi Chang, Chun-Yu Tsai

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This paper is focused on the research of imprinting and replica molding of quasi-grey scale soft mold curved surface microstructure mold. In this paper, a magnetic photocuring forming system is first developed and built independently, then the magnetic curved surface microstructure soft mode is created; moreover, the magnetic performance of the magnetic curved surface at different heights is tested and recorded, and through experimentation and simulation, the magnetic curved surface microstructure soft mold is used in the research of quasi-grey scale soft mold curved surface microstructure imprinting and replica molding. The experimental results show that, under different surface curvatures and voltage control conditions, different quasi-grey scale array microstructures take shape. In addition, this paper conducts research on the imprinting and replica molding of photoresist composite magnetic powder in order to discuss the forming performance of magnetic photoresist, and finally, the experimental result is compared with the simulation to obtain more accurate prediction and results. This research is predicted to provide microstructure component preparation technology with heterogeneity and controllability, and is a kind of valid shaping quasi-grey scale microstructure manufacturing technology method.

Keywords: soft mold, magnetic, microstructure, curved surface

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Authors: Marcelle Muriel Domkam Tchunkam, Rolin Feudjio

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This work investigates the ultrastructure, physicochemical and thermal properties evaluation of Palm Kernel Shells (PKS). PKS Tenera waste samples were obtained from a palm oil mill in Dizangué Sub-Division, Littoral region of Cameroon, while PKS Dura waste samples were collected from the Institute of Agricultural Research for Development (IRAD) of Mbongo. A sodium hydroxide solution was used to wash the shells. They were then rinsed by demineralised water and dried in an oven at 70 °C during 72 hours. They were then grounded and sieved to obtained powders from 0.04 mm to 0.45 mm in size. Transmission Electron Microscopy (TEM) and Surface Electron Microscopy (SEM) were used to characterized powder samples. Chemical compounds and elemental constituents, as well as thermal performance were evaluated by Van Soest Method, TEM/EDXA and SEM/EDS techniques. Thermal characterization was also performed using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). Our results from microstructural analysis revealed that most of the PKS material is made of particles with irregular morphology, mainly amorphous phases of carbon/oxygen with small amounts of Ca, K, and Mg. The DSC data enabled the derivation of the materials’ thermal transition phases and the relevant characteristic temperatures and physical properties. Overall, our data show that PKS have nanopores and show potential in 3D printing and membrane filtration applications.

Keywords: DSC, EDXA, palm kernel shells, SEM, TEM

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Authors: Abdulmagid A. Khattabi, Abdul Fatah M. Emhamed

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The steel alloy Introduced after becoming carbon-steel does not meet the requirements of engineering industry; and it cannot be obtained tensile strength from carbon-steel higher than (700MPa), the low alloy steel enters in a lot of heavy engineering equipment parts, molds, agricultural equipment and other industry. In addition, that may be exposed to in-service failure, which may require returned to work, to do the repairs or maintenance by one of the welding methods available. The ability of steel weld determined through palpation of the cracks, which can reduce by many ways. These ways are often expensive and difficult to implement, perhaps the control to choose the type of electrode welding user is one of the easiest and least expensive applications. It has been welding the steel low alloys high resistance by manual metal arc (MMA), and by using a set of welding electrodes which varying in chemical composition and in their prices as well and test their effect on tensile strength. Results showed that using the poles of welding, which have a high proportion of iron powder and low hydrogen. The Tensile resistance is (484MPa) and the weld joint efficiency was (56.9%), but when (OK 47.04) electrode was used the tensile strength increased to (720MPa) and the weld joint efficiency to (84.7%). Using the cheapest electrode (OK 45.00) the weld joint efficiency did not exceed (24.2%), but when using the most expensive electrode (OK 91.28) the weld joint efficiency is (38.1%).

Keywords: steel low alloys high resistance, electrodes welding, tensile test

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Authors: Amina Adala, Nadra Debbache, Tahar Sehili

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Coordination polymers and uniformly {[Zn(II)(BIPY)(Pht)]n} (1), {[Zn (HYD)(Pht)]n} (2) (BIPY = 4,4’ bipyridine, Pht = terephtalic acid, HYD = 8-hydroxyquinoline) have been successfully synthesized by a hydrothermal process using aqueous zinc solution. The as-prepared compounds phases were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy, UV-visible spectroscopy, thermogravimetric analysis (TGA), and the electrochemistry study by the voltammetry cyclic. The results showed a crystalline phase for CP1 however, CP2 requires recrystallization; the FTIR showed the presence of characteristic bands of all ligands; besides that, TGA shows thermal stability up to 300°C. The electrochemistry study showed a good charge transfer between the ligands and Zn metal for the two components. UV-Vis measurement showed strong absorption in a wide range from UV to visible light with a band gap of 2.69 eV for CP1 and 2.56 eV for CP2, smaller than that of ZnO. This represents an alternative to using ZnO. The Ibuprofen IBP decomposition kinetics of 5.10⁻⁵ mol.L⁻¹ under solar and artificial light were studied for different irradiation conditions. Good photocatalytic properties were observed due to their high surface area.

Keywords: metal-organic frameworks, photocatalysis, photodegradation, organic pollutant, ibuprofen

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Authors: Eman Alzahrani

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Efficient extraction of proteins by removing interfering materials is necessary in proteomics, since most instruments cannot handle such contaminated sample matrices directly. In this study, chitosan-coated magnetic nanoparticles (CS-MNPs) for purification of myoglobin were successfully fabricated. First, chitosan (CS) was prepared by a deacetylation reaction during its extraction from shrimp-shell waste. Second, magnetic nanoparticles (MNPs) were synthesised, using the coprecipitation method, from aqueous Fe2+ and Fe3+ salt solutions by the addition of a base under an inert atmosphere, followed by modification of the surface of MNPs with chitosan. The morphology of the formed nanoparticles, which were about 23 nm in average diameter, was observed by transmission electron microscopy (TEM). In addition, nanoparticles were characterised using X-ray diffraction patterns (XRD), which showed the naked magnetic nanoparticles have a spinel structure and the surface modification did not result in phase change of the Fe3O4. The coating of MNPs was also demonstrated by scanning electron microscopy (SEM) analysis, energy dispersive analysis of X-ray spectroscopy (EDAX), and Fourier transform infrared (FT-IR) spectroscopy. The adsorption behaviour of MNPs and CS-MNPs towards myoglobin was investigated. It was found that the difference in adsorption capacity between MNPs and CS-MNPs was larger for CS-MNPs. This result makes CS-MNPs good adsorbents and attractive for using in protein extraction from biological samples.

Keywords: chitosan, magnetic nanoparticles, coprecipitation, adsorption

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Authors: ChoLiang Chung, YuMin Chen

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C-doped TiO2 nanofibers were prepared by electrospinning successfully. Different amounts of carbon were added into the nanofibers by using chitosan, aiming to shift the wave length that is required to excite the photocatalyst from ultraviolet light to visible light. Different amounts of carbon and different atmosphere fibers were calcined at 500oC, and the optical characteristic of C-doped TiO2 nanofibers had been changed. characterizes of nanofibers were identified by X-Ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FE-SEM), UV-vis, Atomic Force Microscope (AFM), and Fourier Transform Infrared Spectroscopy (FTIR). The XRD is used to identify the phase composition of nanofibers. The morphology of nanofibers were explored by FE-SEM and AFM. Optical characteristics of absorption were measured by UV-Vis. Three dimension surface images of C-doped TiO2 nanofibers revealed different effects of processing. The results of XRD showed that the phase of C-doped TiO2 nanofibers transformed to rutile phase and anatase phase successfully. The results of AFM showed that the surface morphology of nanofibers became smooth after high temperature treatment. Images from FE-SEM revealed the average size of nanofibers. UV-vis results showed that the band-gap of TiO2 were reduced. Finally, we found out C-doped TiO2 nanofibers can change countenance of nanofiber and make it smoother.

Keywords: carbon, TiO2, chitosan, electrospinning

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Authors: Wen-Bin Liau, Wan-Ting Wang, Chiang-Jen Hsiao, Sheng-Mao Tseng

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In this paper, an interesting and easy method to prepare one-dimensional nanostructured polyaniline/dendritic silver composites is reported. It is well known that the morphology of metal particle is a very important factor to influence the properties of polymer-metal composites. Usually, the dendritic silver is prepared by kinetic control in reduction reaction. It is not a thermodynamically stable structure. It is the goal to reduce silver ion to dendritic silver by polyaniline polymer via kinetic control and form one-dimensional nanostructured polyaniline/dendritic silver composites. The preparation is a two steps sequential reaction. First step, the polyaniline networks composed of nano fibrillar polyaniline are synthesized from aniline monomers aqueous with ammonium persulfate as the initiator at room temperature. In second step, the silver nitrate is added into polyaniline networks dispersed in deionized water. The dendritic silver is formed via reduction by polyaniline networks under the kinetic control. The formation of polyaniline is discussed via transmission electron microscopy (TEM). Nanosheets, nanotubes, nanospheres, nanosticks, and networks are observed via TEM. Then, the mechanism of formation of one-dimensional nanostructured polyaniline/dendritic silver composites is discussed. The formation of dendritic silver is observed by TEM and X-ray diffraction.

Keywords: 1D nanostructured polyaniline, dendritic silver, synthesis

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Authors: Qasem Drmosh, Zain Yamai, Amar Mohamedkhair, Abdulmajid Hendi

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In recent years, there has been a growing interest in the reduction of the nitrogen oxides NOx (NO2, NO) gases resulting from automotive or combustion emissions. Recently, metal additives in nanometer dimension onto the surface of SnO2 nanorods, nanowires and nanotubes sensitizer to further increase the sensor response have been used. In contrast, there is a lack study focused on modifying the surface of SnO2 thin films by nanoparticles. The challenge in case of thin films is how to fabricate these nanoparticles on the surfaces in cost-effective method, high purity as well as without hampering electrical and topographical properties. Here in this report, a simple and facile strategy has been demonstrated to acquire high sensitive and fast response NO2 gas sensor. Structural, electrical, morphological, optical, and compositional properties of the fabricated sensors were investigated through different analytical technique including X-ray diffraction (XRD), Field emission scanning emission microscope (FESEM) and X-ray photoelectron spectroscopy (XPS). The sensing performance of the prepared sensors are studied at different temperatures for various concentrations of NO2 and compared with pristine SnO2 film.

Keywords: NO2 sensor, SnO2, sputtering, thin films

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Authors: Ramovatar, Neeraj Panwar

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Lead free Ba₀.₉₈Ca₀.₀₂SnxTi₁₋ₓO₃ (x = 0.01 and 0.05 mole %) ferroelectric ceramics have been synthesized by the solid-state reaction method with sintering at 1400 °C for 2 h. The room temperature x-ray diffraction (XRD) patterns identified the tetragonal phase for x = 0.01 composition whereas co-existence of tetragonal and orthorhombic phases for x =0.05 composition. Raman spectroscopy results corroborated with the XRD results at room temperature. The maximum dielectric properties (ɛm ~ 8591, tanδ ~ 0.018) were obtained for the compound with x = 0.01 at 5 kHz. Further, the tetragonal to cubic (TC) transition temperature was observed at 122 °C and 102 °C for the ceramics with x =0.01 and x = 0.05, respectively. The temperature dependent P-E loops also revealed the existence of TC at these particular temperature values. The energy storage density (Ed) of both compounds was calculated from room temperature P – E loops at an applied electric field of 20 kV/cm. The maximum Ed ~ 224 kJ/m³ was achieved for the sample with x = 0.01 as compared to 164 kJ/m³ for the x =0.05 composition. The value of Ed is comparable to other BaTiO₃ based lead free ferroelectric systems. Impedance spectroscopy analysis exhibited the bulk and grain boundary contributions above 300 °C under the frequency range 100 Hz to 1 MHz. The above properties make these ceramics suitable for energy storage devices.

Keywords: dielectric properties, energy storage properties, impedance spectroscopy, lead free ceramics

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda

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In this report, the impact of Gd³⁺ substitution in ZnFe₂O₄ spinel ferrite nanoparticles on structural, optical and magnetic properties was investigated. ZnFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) nanoparticles were synthesized by honey-mediated sol-gel combustion method. X-ray diffraction, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy confirmed the formation of cubic spinel ferrite crystal structure. The morphology and elemental analysis were studied using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. UV-Visible reflectance spectroscopy revealed band gap variation with concentration of Gd³⁺ substitution in ZnFe₂O₄ nanoparticles. Magnetic property was studied using vibrating sample magnetometer at room temperature. The synthesized spinel ferrite nanoparticles showed ferromagnetic behaviour. The evaluated magnetic parameters such as saturation magnetization, coercivity and remanence showed variation with Gd³⁺ substitution in spinel ferrite nanoparticles. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: sol-gel combustion method, nanoparticles, magnetic property, optical property

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Authors: A. Al-Juboori, D. Wexler, H. Li, H. Zhu, C. Lu, A. McCusker, J. McLeod, S. Pannila, Z. Wang

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Squats are a type railhead defect related to rolling contact fatigue (RCF) damage and are considered serious problem affecting a wide range of railway networks across the world. Squats can lead to partial or complete rail failure. Formation mechanics of squats on the surface of rail steel is still a matter of debate. In this work, structural and microstructural observations from ex-service damaged rail both confirms the phases present in white etching layer (WEL) regions and relationship between cracking in WEL and squat defect formation. XRD synchrotron results obtained from the top surfaces of rail regions containing both WEL and squat defects reveal that these regions contain both martensite and retained austenite. Microstructural analysis of these regions revealed the occurrence cracks extending from WEL down into the rail through the squat region. These findings obtained from field rail specimen support the view that WEL contains regions of austenite and martensitic transformation product, and that cracks in this brittle surface layer propagate deeper into the rail as squats originate and grow.

Keywords: squat, white etching layer, rolling contact fatigue, synchrotron diffraction

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Authors: Angie Quevedo, Juan Bussi, Nestor Tancredi, Juan Fajardo-Díaz, Florentino López-Urías, Emilio Muñóz-Sandoval

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In this work, we study the carbon nanotubes (CNTs) formation by catalytic chemical vapor deposition (CCVD) over a catalyst with 20 % of Ni supported over La₂Zr₂O₇ (Ni20LZO). The high C solubility of Ni made it one of the most used in CNTs synthesis. Nevertheless, Ni presents also sintering and coalescence at high temperature. These troubles can be reduced by choosing a suitable support. We propose La₂Zr₂O₇ as for this matter since the incorporation of Ni by co-precipitation and calcination at 900 °C allows a good dispersion and interaction of the active metal (in the oxidized form, NiO) with this support. The CCVD was performed using 1 g of Ni20LZO at 950 °C during 30 min in Ar:H₂ atmosphere (2.5 L/min). The precursor, benzylamine, was added by a nebulizer-sprayer. X ray diffraction study shows the phase separation of NiO and La₂Zr₂O₇ after the calcination and the reduction to Ni after the synthesis. Raman spectra show D and G bands with a ID/IG ratio of 0.75. Elemental study verifies the incorporation of 1% of N. Thermogravimetric analysis shows the oxidation process start at around 450 °C. Future studies will determine the application potential of the samples.

Keywords: N doped carbon nanotubes, catalytic chemical vapor deposition, nickel catalyst, bimetallic oxide

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Authors: Said Sair, Hanane Ait Ousaleh, Ilyas Belghazi, Othmane Amadine

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Plastic waste has become a major environmental issue, driving the need for innovative solutions to convert it into valuable resources. This study explores the catalytic pyrolysis of plastic waste to produce hydrogen, using zeolite catalysts as a key component in the process. Various zeolites, including types X, A, and P, are synthesized and characterized through X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), Brunauer–Emmett–Teller (BET) surface area analysis, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). These techniques are employed to assess the structural and chemical properties of the catalysts. Catalytic pyrolysis experiments are performed under different conditions, including variations in temperature, catalyst loading, and reaction time, to optimize hydrogen production. The results demonstrate that the choice of zeolite catalyst significantly impacts plastic waste conversion efficiency into hydrogen. This research contributes to advancing circular economy principles by providing an effective method for plastic waste management and clean energy production, promoting environmental sustainability.

Keywords: hydrogen production, plastic waste, zeolite catalysts, catalytic pyrolysis, circular economy, sustainable energy

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Authors: S. Barbaqadze, M. Goderdzishvili, E. Mosidze, L. Lomtadze, V. Mshvildadze, L. Bakuridze, D. Berashvili, A. Bakuridze

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This paper focuses on the formulation of phytobiotic designated for further implantation in poultry farming. Composition was meant to be water-soluble powder containing antibacterial essential oils. The development process involved Thyme, Monarda and Clary sage essential oils. The antimicrobial activity of essential oils composite was meant to be tested against gram-negative and gram-positive bacterial strains. The results are processed using the statistical program Sigma STAT. To make essential oils composition water soluble surfactants were added to them. At the first stage of the study, nine options for the optimal composition of essential oils and surfactants were developed. The effect of the amount of surfactants on the essential oils composition solubility in water has been investigated. On the basis of biopharmaceutical studies, the formulation of phytobiotic has been determined: Thyme, monarda and clary sage essential oils 2:1:1 - 100 parts; Licorice extract 5.25 parts and inhalation lactose 300 parts. A technology for the preparation of phytobiotic has been developed and a technological scheme for the preparation of phytobiotic has been made up. The research was performed within the framework of the grant project CARYS-19-363 funded be the Shota Rustaveli National Science Foundation of Georgia.

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

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Authors: Muhamad Syafiq Hakimi Kamaruddin, Norhidayah Suleiman

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Ginger extracts (Zingiber officinale Rosc.) have been attributed therapeutic properties primarily as antioxidant, anticancer, and anti-inflammatory properties. Conventional extractions including Soxhlet and maceration are commonly used to extract the bioactive compounds from plant material. Nevertheless, high energy consumption and being non-environmentally friendly are the predominant limitations of the conventional extractions method. Herein, green technology, namely supercritical carbon dioxide (scCO2) extraction, is used to study process variables' effects on extract yields. Herein, green technology, namely supercritical carbon dioxide (scCO2) extraction, is used to study process variables' effects on extract yields. A pressure (10-30 MPa), temperature (40-60 °C), and median particle size (300-600 µm) were conducted at a CO2 flow rate of 0.9 ± 0.2 g/min for 120 mins. The highest overall yield was 4.58% obtained by the scCO2 extraction conditions of 300 bar and 60 °C with 300µm of ginger powder for 120 mins. In comparison, the yield of the extract was increased considerably within a short extraction time. The results show that scCO2 has a remarkable ability over ginger extract and is a promising technology for extracting bioactive compounds from plant material.

Keywords: conventional, ginger, non-environmentally, supercritical carbon dioxide, technology

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Authors: J. Ptačinová, J. Ďurica, P. Jurči, M Kusý

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Ledeburitic tool steel Vanadis 6 has been subjected to sub-zero treatment (SZT) at -140 °C and -196 °C, for different durations up to 48 h. The microstructure and hardness have been examined with reference to the same material after room temperature quenching, by using the light microscopy, scanning electron microscopy, X-ray diffraction, and Vickers hardness testing method. The microstructure of the material consists of the martensitic matrix with certain amount of retained austenite, and of several types of carbides – eutectic carbides, secondary carbides, and small globular carbides. SZT reduces the retained austenite amount – this is more effective at -196 °C than at -140 °C. Alternatively, the amount of small globular carbides increases more rapidly after SZT at -140 °C than after the treatment at -140 °C. The hardness of sub-zero treated material is higher than that of conventionally treated steel when tempered at low temperature. Compressive hydrostatic stresses are developed in the retained austenite due to the application of SZT, as a result of more complete martensitic transformation. This is also why the population density of small globular carbides is substantially increased due to the SZT. In contrast, the hardness of sub-zero treated samples decreases more rapidly compared to that of conventionally treated steel, and in addition, sub-zero treated material induces a loss the secondary hardening peak.

Keywords: microstructure, Vanadis 6 tool steel, sub-zero treatment, carbides

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Authors: Kashif Jabbar

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Milk adulteration is a global concern, and the current study was plan to synthesize Selenium nanoparticles by green method using plant extract of garlic, Allium Sativum, and to characterize Selenium nanoparticles through different analytical techniques and to apply Selenium nanoparticles as fast and easy technique for the detection of salicylic acid in milk. The highly selective, sensitive, and quick interference green synthesis-based sensing of possible milk adulterants i.e., salicylic acid, has been reported here. Salicylic acid interacts with nanoparticles through strong bonding interactions, hence resulting in an interruption within the formation of selenium nanoparticles which is confirmed by UV-VIS spectroscopy, scanning electron microscopy, and x-ray diffraction. This interaction in the synthesis of nanoparticles resulted in transmittance wavelength that decrease with the increasing amount of salicylic acid, showing strong binding of selenium nanoparticles with adulterant, thereby permitting in-situ fast detection of salicylic acid from milk having a limit of detection at 10-3 mol and linear coefficient correlation of 0.9907. Conclusively, it can be draw that colloidal selenium could be synthesize successfully by garlic extract in order to serve as a probe for fast and cheap testing of milk adulteration.

Keywords: adulteration, green synthesis, selenium nanoparticles, salicylic acid, aggregation

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Authors: M. Nagaraja, H. M. Mahesh, K. Rajanna, M. Z. Kurian, J. Manjanna

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In recent years, composites of conjugated polymers with fullerenes (C60) has attracted considerable scientific and technological attention in the field of organic electronics because they possess a novel combination of electrical, optical, ferromagnetic, mechanical and sensor properties. These properties represent major advances in the design of organic electronic devices. With the addition of C60 in the conjugated polymer matrix, the primary photo-excitation of the conjugated polymer undergoes an ultrafast electron transfer, and it has been demonstrated that fullerene molecules may serve as efficient electron acceptors in polymeric solar cells. The present paper includes the systematic studies on the effect of electrical, structural and sensor properties of polyaniline (PANI) matrix by the presence of C60. Polyaniline-fullerene (PANI/C60) composite is prepared by the introduction of fullerene during polymerization of aniline with ammonium persulfate and dodechyl benzene sulfonic acid as oxidant and dopant respectively. FTIR spectroscopy indicated the interaction between PANI and C60. X-ray diffraction proved the formation of a PANI/C60 complex. SEM image shows the highly branched chain structure of the PANI in the presence of C60. The conductivity of the PANI/C60 was found to be more than ten orders of magnitude over the pure PANI.

Keywords: conductivity, fullerene, nanocomposite, polyaniline

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Authors: Marzieh Joda, Narges Fallah, Neda Afsham

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Graphite-supported two different of morphology α and β -Ni (OH)₂ electrodes were prepared by electrochemical deposition at appropriate potentials with regard to Ni (II)/Ni (III) redox couple under alkaline and acidic conditions, respectively, for selective oxidation of ammonia to nitrogen in the direct electro-oxidation process. Cyclic voltammetry (CV) of the electrolyte containing NH₃ indicated mediation of electron transfer by Ni (OH)₂ and the electrode surface was analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectrometer (RS), and X-ray photoelectron spectroscopy (XPS). Results of surface characterization indicated the presence of α polymorphs which is the stable phase of Ni (OH)₂ /Graphite. Cyclic voltammograms gave information on the nature of electron transfer between nitrogen species and working electrode and revealed that the potential has depended on both nature ammonia oxidation and that of concentration. The mechanism of selective ammonia conversion to nitrogen and byproducts, namely NO₂- and NO₃- was established by Cyclic voltammograms and current efficiency. The removal efficiency and selective conversion of ammonia (0.1 M KNO₃ + 0.01 M Ni(NO₃)₂, pH 11, 250°C) on Nickel Oxide-hydroxide /Graphite was determined based on potential controlled experiments.

Keywords: Electro deposition, Nickel oxide-hydroxide, Nitrogen selectivity, Ammonia oxidation

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Authors: Anant Pandey, Kanika Sharma, Vibha Chopra, Shaila Bahl, Pratik Kumar, S. P. Lochab, Birendra Singh

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This paper reports the thermoluminescence (TL) properties of nanocrystalline CaSO₄ activated by Ce, Sm, and Dy. TL properties are investigated by chiefly changing the dopant element and also by varying the concentration of the dopant elements (from 0.05 mol % to 0.5 mol %) so as to establish the optimized dopant concentration for each of the activators. The method of salt preparation used is the typical chemical co-precipitation method and the technique used for characterization of the prepared samples is the X-Ray Diffraction (XRD) technique. Further, the phosphors are irradiated with gamma radiation from Co-60 (1.25 MeV) source (dose range- 30 Gy to 500 Gy). The optimized concentration (vis-a-vis TL peak intensity) of activator for CaSO₄:Ce is found to be 0.2 mol %, for CaSO₄:Sm it is 0.1 mol % and for CaSO₄:Dy it is 0.2 mol %. Further, the primary study of the TL response curves for all the three phosphors confirms linearity in the studied dose range (i.e., 30 Gy to 500 Gy). Finally, CaSO₄:Dy was also studied for its energy dependence property which plays an important role in defining the utility of a phosphor for dosimetric applications. The range of doses used for the energy dependence study was from 30 Gy to 500 Gy from Cs-137 (0.662 MeV). The nano-phosphors showed potential to be used as radiation dosimeter in the studied range of gamma radiation and thus must be studied for a wider range of doses.

Keywords: gamma radiation, nanocrystalline, radiation dosimetry, thermoluminescence

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Authors: Alireza Bahramian

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High-purity TiO₂ nanoparticles (NPs) with size ranging between 50 nm and 100 nm are synthesized from titanium slag through sulphate route under sonochemical procedure. The effect of dissolution parameters such as the sulfuric acid/slag weight ratio, caustic soda concentration, digestion temperature and time, and initial particle size of the dried slag on the extraction efficiency of TiO₂ and removal of iron are examined. By optimizing the digestion conditions, a rutile TiO₂ powder with surface area of 42 m²/g and mean pore diameter of 22.4 nm were prepared. A thermo-kinetic analysis showed that the digestion temperature has an important effect, while the acid/slag weight ratio and initial size of the slag has a moderate effect on the dissolution rate. The shrinking-core model including both chemical surface reaction and surface diffusion is used to describe the leaching process. A low value of activation energy, 38.12 kJ/mol, indicates the surface chemical reaction model is a rate-controlling step. The kinetic analysis suggested a first order reaction mechanism with respect to the acid concentrations.

Keywords: TiO₂ nanoparticles, titanium slag, dissolution rate, sonochemical method, thermo-kinetic study

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Authors: A. Alvaredo , R. Guzman De Villoria, P. Castell, Juan P. Fernandez-Blazquez

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Since graphene was discovered in 2004, has been considered as superb material, due to its outstanding mechanical, electrical and thermal properties. Graphene has been incorporated as reinforcement in several high performance polymers in order to obtain a good balance of properties and to get new properties as thermal or electric conductivity. As well known, the properties of semicrystalline polymer and its composites depends heavily on degree of crystallinity. In this context, our research group has studied the crystallization behavior from amorphous state of PEEK/GNP composites. The monitoring of cold crystallization processes studied by time-resolved simultaneous wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS). These techniques allowed to get an extremely relevant information about the evolution of the morphology of the PEEK/GNP composites. In addition, the thermal evolution of cold crystallization was followed by differential scanning calorimetry (DSC) as well. The experimental results showed changes in crystallization kinetics and c parameter unit cell when adding graphene. The main aim of this work is to produce PEEK/GNP composites and characterize their morphology, unit cell parameters and crystallization kinetic.

Keywords: PEEK, graphene, synchrotron, cold crystallization

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Authors: Rabah Bensaha, Badreeddine Toubal

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Un-doped TiO2, Co single doped TiO2 and (Cu-Co) co-doped TiO2 thin films have been growth on silicon substrates by the sol-gel dip coating technique. We mainly investigated both effects of the dopants and annealing temperature on the structural, optical and electrical properties of TiO2 films using X-ray diffraction (XRD), Raman and FTIR spectroscopy, Atomic force microscopy (AFM), Scanning electron microscopy (SEM), UV–Vis spectroscopy. The chemical compositions of Co-doped and (Cu-Co) co-doped TiO2 films were confirmed by XRD, Raman and FTIR studies. The average grain sizes of CoTiO3-TiO2 nanocomposites were increased with annealing temperature. AFM and SEM reveal a completely the various nanostructures of CoTiO3-TiO2 nanocomposites thin films. The films exhibit a high optical reflectance with a large band gap. The highest electrical conductivity was obtained for the (Cu-Co) co-doped TiO2 films. The polyhedral surface morphology might possibly improve the surface contact between particle sizes and then contribute to better electron mobility as well as conductivity. The obtained results suggest that the prepared TiO2 films can be used for optoelectronic applications.

Keywords: sol-gel, TiO2 thin films, CoTiO3-TiO2 nanocomposites films, Electrical conductivity

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Authors: Y. Boudjadja, A. Amira, A. Saoudel, A. Varilci, S. P. Altintas, C. Terzioglu

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In this work, we report the effect of Y3+ doping on structural, mechanical and electrical properties of Bi-2202 phase. Samples of Bi2Sr1.9Ca0.1-xYxCu2O7+δ with x = 0, 0.025, 0.05, 0.075 and 0.1 are elaborated in air by conventional solid state reaction and characterized by X-Ray Diffraction (XRD), Scanning Electronic Microscopy (SEM) combined with EDS spectroscopy, density, Vickers micro-hardness and resistivity measurements. A good correlation between the variations of the bulk density and the Vickers micro-hardness with doping is obtained. The SEM photograph shows that the samples are composed of grains with a flat shape that characterizes the Bi-based cuprates. Quantitative EDS analysis confirms the reduction of Ca content and the increase of Y content when x is increased. The variation of resistivity with temperature shows that only samples with x = 0, 0.025 and 0.05 present an onset transition to the superconducting state. The higher onset transition temperature is obtained for x = 0.025 and is about 93.62 K. The transition is wide and is realized in two steps confirming then the presence of the low Tc Bi-2201 phase in the samples. For x = 0.075 and 0.1, a transition to a semiconducting state is seen at low temperatures. Some physical parameters are extracted from these curves and discussed.

Keywords: Bi-2202 phase, doping, structure, mechanical and electrical properties

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Authors: Edgar Ochoa, G. Torres-Villasenor

Abstract:

Superplastic deformation is shown by materials with a fine grain size, usually less than 10 μm, when they are deformed within the strain rate range 10-5 10-1 s-1 at temperatures greater than 0.5Tm, where Tm is the melting point in Kelvin. According to the constitutive equation for superplastic flow, refinement of the grain size would be expected to increase the optimum strain rate and decrease the temperature required for superplastic flow. Ribbons of eutectic Ag-Cu and Bi-Cd alloys were manufactured by using a single roller melt-spinning technique to obtain a fine grain structure for later test in superplastic regime. The eutectics ribbons were examined by scanning electron microscopy and X-Ray diffraction, and the grain size was determined using the image analysis software ImageJ. The average grain size was less than 1 μm. Tensile tests were carried out from 10-4 to 10-1 s-1, at room temperature, to evaluate the superplastic behavior. The largest deformation was shown by the Bi-Cd eutectic ribbons, Ɛ=140 %, despite that these ribbons have a hexagonal unit cell. On the other hand, Ag-Cu eutectic ribbons have a minor grain size and cube unit cell, however they showed a lower deformation in tensile test under the same conditions than Bi-Cd ribbons. This is because the Ag-Cu grew in a strong cube-cube orientation relationship.

Keywords: eutectic ribbon, fine grain, superplastic deformation, cube-cube orientation

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Authors: Asiful H. Seikh, Jabair A. Mohammed, Ubair A. Samad, Mohammad A. Alam, Saeed M. Al-Zahrani, El-Sayed M. Sherif

Abstract:

Three coating formulations were fabricated by incorporating different percentages of MIO (micaceous iron oxide ) (1, 2, and wt%) with ball-milled nanocrystalline Al (2 wt%) particles, which was optimized earlier. These coatings were characterized by means of different methods, namely, SEM, TGA, pendulum hardness, scratch test, and nano-indentation. The EIS measurements were carried out to report the effect of adding MIO powder in fabricated coatings on their corrosion behavior in 3.5 wt% NaCl solutions. In order to report the effect of immersion time on the corrosion and degradation of the prepared coatings, the EIS data were also acquired after various exposure periods of time, i.e., 1 h, 7 d, 14 d, 21 d, and 30 d in the test chloride solution. It has been found that the obtained EIS data for the fabricated coatings proved that the presence of 2% MIO provided the highest corrosion resistance amongst all coatings and that effect was recorded after all immersion periods of time. But, the MIO-incorporated coatings have less corrosion resistance than Al based epoxy coatings. It was also shown that with prolonged immersion, the resistance to corrosion declined after 7d, then with a longer period of immersion, i.e. 14 d, 21 d, and 30 d increases the resistance to corrosion by forming oxide products on the coatings surface. The results obtained from both mechanical and electrochemical testing confirmed that the fabricated coating with 2 wt% Al exhibited better hardness and higher resistance to corrosion as compared to coatings with 1 wt% Al and 3 wt% Al.

Keywords: epoxy coatings, nanomaterials, corrosion resistance, EIS, nanoindentation

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Authors: Pheiroijam Pooja, P. Chinnamuthu

Abstract:

A novel vertical 1D In2O3/TiO2 nanocolumn (NC) axial heterostructure has been successfully synthesized using Glancing Angle Deposition (GLAD) technique inside E-Beam Evaporator chamber. Field emission scanning electron microscope (FESEM) has been used to evaluate the morphology of the structure grown. The estimated length of In2O3/TiO2 NC is ~250 nm and ~300nm for In2O3 and TiO2 respectively with diameter ~60-90 nm. The surface of the heterostructure is porous in nature which can affect the interfacial wettability properties. The grown structure has been further characterized using X-ray Diffraction (XRD) and UV-Visible absorption measurement. The polycrystalline nature of the sample has been examined using XRD with prominent peaks obtained with phase (101) for anatase TiO2 and (211) for In2O3. Here, 1D axial heterostructure NC thus favors efficient segregation of photo-excited carriers due to their type II band alignment between the constituent materials. Moreover, the 1D nanostructure is known for their large surface area and excellent ionic charge transport property. On exposure to UV light illumination, the surface properties of In2O3/TiO2 NC changes whereby the hydrophobic nature of the heterostructure changes to hydrophilic. As a result, the reversible surface wettability of heterostructure on interaction with UV light can give potential applications as antifogging and self-cleaning surfaces.

Keywords: GLAD, heterostructure, In2O3/TiO2 NC, surface wettability

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Authors: Yu-Chen Chang, Yen-Ping Peng, Wei-Yu Chen, Ku-Fan Chen

Abstract:

Contamination of soil and groundwater has become a serious and widespread environmental problem. In this study, sustained-release persulfate tablets were developed using persulfate powder and a modified cellulose binder for organic-contaminated groundwater remediation. Conventional cement-based persulfate-releasing materials were also synthesized for the comparison. The main objectives of this study were to: (1) evaluate the release rates of the remedial tablets; (2) obtain the optimal formulas of the tablets; and (3) evaluate the effects of the tablets on the subsurface environment. The results of batch experiments show that the optimal parameter for the preparation of the persulfate-releasing tablet was persulfate:cellulose = 1:1 (wt:wt) with a 5,000 kg F/cm2 of pressure application. The cellulose-based persulfate tablet was able to release 2,030 mg/L of persulfate per day for 10 days. Compared to cement-based persulfate-releasing materials, the persulfate release rates of the cellulose-based persulfate tablets were much more stable. Moreover, since the tablets are soluble in water, no waste will be produced in the subsurface. The results of column tests show that groundwater flow would shorten the release time of the tablets. This study successfully developed unique persulfate tablets based on green remediation perspective. The efficacy of the persulfate-releasing tablets on the removal of organic pollutants needs to be further evaluated. The persulfate tablets are expected to be applied for site remediation in the future.

Keywords: sustained-release persulfate tablet, modified cellulose, green remediation, groundwater

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Authors: Nagarjuna Remalli, Robert Brandt

Abstract:

Down-sizing of combustion engines in automobiles are prevailed owing to required increase in efficiency. This leads to a stress increment on valve springs, which affects their intended function due to an increase in relaxation. High strength martensitic steels are used for valve spring applications. Recent investigations unveiled that low temperature creep (LTC) in martensitic steels obey a logarithmic creep law. The exhaustion theory links the logarithmic creep behavior to an activation energy which is characteristic for any given time during creep. This activation energy increases with creep strain due to barriers of low activation energies exhausted during creep. The assumption of the exhaustion theory is that the material is inhomogeneous in microscopic scale. According to these assumptions it is anticipated that small obstacles (e. g. ε–carbides) having a wide range of size distribution are non-uniformly distributed in the materials. X-ray diffraction studies revealed the presence of ε–carbides in high strength martensitic steels. In this study, high strength martensitic steels that are crept in the temperature range of 75 – 150 °C were investigated with the aid of a transmission electron microscope for the evidence of an inhomogeneous distribution of obstacles having different size to examine the validation of exhaustion theory.

Keywords: creep mechanisms, exhaustion theory, low temperature creep, martensitic steels

Procedia PDF Downloads 262