Search results for: Photoluminescence Spectroscopy (PL) and Field Effect Scanning electron microscopy (FESEM)

Authors: Raees Khan, Sheikh Z. Ul Abidin, Abdul S. Mumtaz, Jie Liu

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The present study is intended to assess gymnosperms pollen flora of Pakistan using Light Microscope (LM) and Scanning Electron Microscopy (SEM) for its taxonomic significance in identification of gymnosperms. Pollens of 35 gymnosperm species (12 genera and five families) were collected from its various distributional sites of gymnosperms in Pakistan. LM and SEM were used to investigate different palyno-morphological characteristics. Five pollen types (i.e., Inaperturate, Monolete, Monoporate, Vesiculate-bisaccate, and Polyplicate) were observed. In equatorial view seven types of pollens were observed, in which ten species were sub-angular, nine species were triangular, six species were perprolate, three species were rhomboidal, three species were semi-angular, two species were rectangular and two species were prolate. While five types of pollen were observed in polar view, in which ten species were spheroidal, nine species were angular, eight were interlobate, six species were circular, and two species were elliptic. Eighteen species have rugulate and 17 species has faveolate ornamentation. Eighteen species have verrucate and 17 have gemmate type sculpturing. The data was analysed through cluster analysis. The study showed that these palyno-morphological features have significance value in classification and identification of gymnosperms. Based on these different palyno-morphological features, a taxonomic key was proposed for the accurate and fast identifications of gymnosperms from Pakistan.

Keywords: gymnosperms, palynology, Pakistan, taxonomy

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Authors: Yuan-Ching Lin, Tian-Yi Huang, Ming-Jhe Hsieh

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In this work, soybean biodiesel was blended with petroleum diesel as testing oils (B2). The tribiological performance of the B2 biodiesel before and after aging was evaluated using a reciprocating cylinder-on-flat wear test rig (Cameron-Plint TE-77) at various temperatures. The worn surface of each tested specimen was observed using a field-emission scanning electron microscope (FESEM). The compositions of the chemical films on each worn surface were determined using an energy dispersive spectrometer (EDS). The experimental results demonstrate that the tribiological behavior of the B2 was superior to that of other testing oils. Furthermore, the aging of biodiesel caused acidification, which resulted in poorer wear performance in the same experimental condition compared with others. The worn morphology of the specimen that was tested in the aged soybean biodiesel exhibited corrosion wear, reflecting low wear resistance.

Keywords: biodiesel, soybean, tribological performance

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Authors: Michael Shandalov, Tzvi Templeman, Michael Schmidt, Itzhak Kelson, Eyal Yahel

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We present a new method to produce a model system for the study of radiation damage in non-radioactive materials. The method is based on homogeneously incorporating 228Th ions in PbS thin films using a small volume chemical bath deposition (CBD) technique. The common way to alloy metals with radioactive elements is by melting pure elements, which requires considerable amounts of radioactive material with its safety consequences such as high sample activity. Controlled doping of the thin films with (very) small amounts (100-200ppm) of radioactive elements such as thorium is expected to provide a unique path for studying radiation damage in materials due to decay processes without the need of sealed enclosure. As a first stage, we developed CBD process for controlled doping of PbS thin films (~100 nm thick) with the stable isotope (t1/2~106 years), 232Th. Next, we developed CBD process for controlled doping of PbS thin films with active 228Th isotope. This was achieved by altering deposition parameters such as temperature, pH, reagent concentrations and time. The 228Th-doped films were characterized using X-ray diffraction, which indicated a single phase material. Film morphology and thickness were determined using scanning electron microscopy (SEM). Energy dispersive spectroscopy (EDS) mapping in the analytical transmission electron microscope (A-TEM), X-ray photoelectron spectroscopy (XPS) depth profiles and autoradiography indicated that the Th ions were homogeneously distributed throughout the films, suggesting Pb substitution by Th ions in the crystal lattice. The properties of the PbS (228Th) film activity were investigated by using alpha-spectroscopy and gamma spectroscopy. The resulting films are applicable for isochronal annealing of resistivity measurements and currently under investigation. This work shows promise as a model system for the analysis of dilute defect systems in semiconductor thin films.

Keywords: thin films, doping, radiation damage, chemical bath deposition

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Authors: Mohamed Abd Elfattah Ibraheem Elghrbawy

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Biodeterioration of cultural heritage is a complex process which is caused by the interaction of many physical, chemical and biological agents; the growth of microorganisms can cause staining, cracking, powdering, disfigurement and displacement of monuments material, which leads to the permanent loss of monuments material. Organisms causing biodeterioration on monuments have usually been controlled by chemical products (biocides). In order to overcome the impact of biocides on the environment, human health and monument substrates, alternative tools such as antimicrobial agents from natural products can be used for monuments conservation and protection. The problem is how to formulate antibacterial agents with high efficiency and low toxicity. Various types of biodegradable metal nanoparticles (MNPs) have many applications in plant extract delivery. So, Nano-encapsulation of metal and natural antimicrobial agents using polymers such as chitosan increases their efficacy, specificity and targeting ability. Green synthesis and characterization of metal nanoparticles such as silver with natural products extracted from some plants having antimicrobial properties, using the ecofriendly method one pot synthesis. Encapsulation of the new synthesized mixture using some biopolymers such as chitosan nanoparticles. The dispersions and homogeneity of the antimicrobial heterogeneous metal nanoparticles encapsulated by biopolymers will be characterized and confirmed by Fourier Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM) and Zeta seizer. The effect of the antimicrobial biopolymer metal nano-formulations on normal human cell lines will be investigated to evaluate the environmental safety of these formulations. The antimicrobial toxic activity of the biopolymeric antimicrobial metal nanoparticles formulations will be will be investigated to evaluate their efficiency towards different pathogenic bacteria and fungi.

Keywords: antimicrobial, biodeterioration, chitosan, cultural heritage, silver

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Authors: Yehia Manawi, Viktor Kochkodan, Muataz Hussien

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In this paper, the effect of adding Arabic Gum (AG) to the dope solutions of polyethersulfone (PES) was studied. The aim of adding AG is to enhance the properties of ultrafiltration membranes such as hydrophilicity, porosity and selectivity. several AG loading (0.1-3.0 wt.%) in PES/ N-Methyl-2-pyrrolidone (NMP) casting solutions were prepared to fabricate PES membranes using phase inversion technique. The surface morphology, hydrophilicity and selectivity of the cast PES/AG membranes were analyzed using scanning electron microscopy and contact angle measurements. The selectivity of the fabricated membranes was also tested by filtration of oil solutions (1 ppm) and found to show quite high removal efficiency. The effect of adding AG to PES membranes was found to increase the permeate flux and porosity as well as reducing surface roughness and the contact angle of the membranes.

Keywords: antifouling, Arabic gum, polyethersulfone membrane, ultrafiltration

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Authors: Saeed Khodabakhshi, Alimorad Rashidi, Ziba Tavakoli, Sajad Kiani, Sadegh Dastkhoon

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Alumina nanoparticles (γ-Al2O3 NPs) were prepared via a new and simple synthetic route and characterized by field emission scanning electron microscope, X-ray diffraction, and Fourier transform infrared spectroscopy. The catalytic activity of prepared γ-Al2O3 NPs was investigated for the one-pot, four-component synthesis of fused tri-heterocyclic compounds containing pyrazole, pyran, and pyrimidine. This procedure has some advantages such as high efficiency, simplicity, high rate and environmental safety.

Keywords: alumina nanoparticles, one-pot, fused tri-heterocyclic compounds, pyran

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Authors: Abdel Ghany F. Shoair, Mai M. A. H. Shanab

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The basic aqueous systems NiSO4.6H₂O / K₂S₂O₈ (PH= 14) or NiSO₄.6H₂O / KBrO₃ (PH = 11.5) were ‎investigated ‎for the ‎catalytic conversion benzyl alcohol and ‎some para-substituted benzyl ‎alcohols to their ‎corresponding ‎acids in 75-97 % yield at room ‎temperature. The active species ‎was isolated and characterized by scanning ‎electron ‎microscopy (SEM), ‎‎transmission electron microscopy (TEM), X-ray ‎powder diffraction, EDX and ‎‎FT-IR ‎techniques and identified as NiO₂ nanoparticles (NPNPs). The SEM and ‎TEM images of nickel peroxide samples show a fine spherical-like ‎aggregation of ‎NiO₂ molecules with a nearly homogeneous partial size and confirm the ‎aggregation's size ‎to ‎be in the range of 2-3 nm. The yields, turnover (TO) and turn ‎over frequencies (TOF) were calculated. ‎It was noticed ‎that the aromatic alcohols ‎containing para-substituted electron donation groups gave better ‎‎yields than ‎those having electron-withdrawing groups. The optimum conditions for this ‎‎catalytic reaction ‎were studied using benzyl alcohol as a model. The mechanism ‎of the ‎catalytic conversion reaction was ‎suggested, in which the produced ‎(NPNPs) convert alcohols ‎to acids in two steps through the formation of the ‎‎corresponding aldehyde. The produced ‎NiO, because of this conversion, is ‎converted again to (NPNPs) by ‎an excess of K₂S₂O₈ or KBrO₃. This ‎catalytic cycle continues ‎until all the substrate is oxidized.

Keywords: Nickel, oxidation, catalysts, benzyl alcohol

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Authors: Abdulqader Alkhouzaam, Hazim Qiblawey, Majeda Khraisheh

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Membrane treatment for desalination and wastewater treatment is one of the promising solutions to affordable clean water. It is a developing technology throughout the world and considered as the most effective and economical method available. However, the limitations of membranes’ mechanical and chemical properties restrict their industrial applications. Hence, developing novel membranes was the focus of most studies in the water treatment and desalination sector to find new materials that can improve the separation efficiency while reducing membrane fouling, which is the most important challenge in this field. Graphene oxide (GO) is one of the materials that have been recently investigated in the membrane water treatment sector. In this work, ultrafiltration polysulfone (PSF) membranes with high antifouling properties were synthesized by incorporating different loadings of GO. High-oxidation degree GO had been synthesized using a modified Hummers' method. The synthesized GO was characterized using different analytical techniques including elemental analysis, Fourier transform infrared spectroscopy - universal attenuated total reflectance sensor (FTIR-UATR), Raman spectroscopy, and CHNSO elemental analysis. CHNSO analysis showed a high oxidation degree of GO represented by its oxygen content (50 wt.%). Then, ultrafiltration PSF membranes incorporating GO were fabricated using the phase inversion technique. The prepared membranes were characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM) and showed a clear effect of GO on PSF physical structure and morphology. The water contact angle of the membranes was measured and showed better hydrophilicity of GO membranes compared to pure PSF caused by the hydrophilic nature of GO. Separation properties of the prepared membranes were investigated using a cross-flow membrane system. Antifouling properties were studied using bovine serum albumin (BSA) and humic acid (HA) as model foulants. It has been found that GO-based membranes exhibit higher antifouling properties compared to pure PSF. When using BSA, the flux recovery ratio (FRR %) increased from 65.4 ± 0.9 % for pure PSF to 84.0 ± 1.0 % with a loading of 0.05 wt.% GO in PSF. When using HA as model foulant, FRR increased from 87.8 ± 0.6 % to 93.1 ± 1.1 % with 0.02 wt.% of GO in PSF. The pure water permeability (PWP) decreased with loadings of GO from 181.7 L.m⁻².h⁻¹.bar⁻¹ of pure PSF to 181.1, and 157.6 L.m⁻².h⁻¹.bar⁻¹ with 0.02 and 0.05 wt.% GO respectively. It can be concluded from the obtained results that incorporating low loading of GO could enhance the antifouling properties of PSF hence improving its lifetime and reuse.

Keywords: antifouling properties, GO based membranes, hydrophilicity, polysulfone, ultrafiltration

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Authors: Soheir Mohamed Fathey

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Biofilms are complex biological communities which are hard to be eliminated by conventional antibiotic administration and implemented in eighty percent of humans infections. Green remedies have been used for centuries and have shown obvious effects in hindering and combating microbial biofilm infections. Nowadays, there has been a growth in the number of researches on the anti-biofilm performance of natural agents such as plant essential oil (EOs) and propolis. In this study, we investigated the antibiofilm performance of various natural agents, including four essential oils (EOs), cinnamon (Cinnamomum cassia), tea tree (Melaleuca alternifolia), and clove (Syzygium aromaticum), as well as propolis versus the biofilm of both Gram-positive pathogenic bacterium Staphylococcus aureus and Gram-negative pathogenic bacterium Pseudomonas aeruginosa which are major human and animal pathogens rendering a high risk due to their biofilm development ability. The antibiofilm activity of the tested agents was evaluated by crystal violet staining assay and detected by scanning electron and fluorescent microscopy. Antibiofilm performance declared a potent effect of the tested products versus the tested bacterial biofilms.

Keywords: biofilm, essential oils, electron microscopy, fluorescent

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Authors: Amir Shafiee Kisomi, Mehrdad Mofidi

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Nowadays, fuel cells as a promising alternative for power source have been widely studied owing to their security, high energy density, low operation temperatures, renewable capability and low environmental pollutant emission. The nanoparticles of core-shell type could be widely described in a combination of a shell (outer layer material) and a core (inner material), and their characteristics are greatly conditional on dimensions and composition of the core and shell. In addition, the change in the constituting materials or the ratio of core to the shell can create their special noble characteristics. In this study, a fast technique for the fabrication of a Pd-Co/G/GCE modified electrode is offered. Thermal decomposition reaction of cobalt (II) formate salt over the surface of graphene/glassy carbon electrode (G/GCE) is utilized for the synthesis of Co nanoparticles. The nanoparticles of Pd-Co decorated on the graphene are created based on the following method: (1) Thermal decomposition reaction of cobalt (II) formate salt and (2) the galvanic replacement process Co by Pd2+. The physical and electrochemical performances of the as-prepared Pd-Co/G electrocatalyst are studied by Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDS), Cyclic Voltammetry (CV), and Chronoamperometry (CHA). Galvanic replacement method is utilized as a facile and spontaneous approach for growth of Pd nanostructures. The Pd-Co/G is used as an anode catalyst for ethanol oxidation in alkaline media. The Pd-Co/G not only delivered much higher current density (262.3 mAcm-2) compared to the Pd/C (32.1 mAcm-2) catalyst, but also demonstrated a negative shift of the onset oxidation potential (-0.480 vs -0.460 mV) in the forward sweep. Moreover, the novel Pd-Co/G electrocatalyst represents large electrochemically active surface area (ECSA), lower apparent activation energy (Ea), higher levels of durability and poisoning tolerance compared to the Pd/C catalyst. The paper demonstrates that the catalytic activity and stability of Pd-Co/G electrocatalyst are higher than those of the Pd/C electrocatalyst toward ethanol oxidation in alkaline media.

Keywords: thermal decomposition, nanostructures, galvanic replacement, electrocatalyst, ethanol oxidation, alkaline media

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Authors: Shadatul Hanom Rashid, Xiaorong Zhou

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Hybrid sol-gel coatings are the blend of both advantages of inorganic and organic networks have been reported as environmentally friendly anti-corrosion surface pre-treatment for several metals, including aluminum alloys. In this current study, Si-Zr hybrid sol-gel coatings were synthesized from (3-glycidoxypropyl)trimethoxysilane (GPTMS), tetraethyl orthosilicate (TEOS) and zirconium(IV) propoxide (TPOZ) precursors and applied on AA6111 aluminum alloy by dip coating technique. The hybrid sol-gel coatings doped with different concentrations of cerium nitrate (Ce(NO3)3) as a corrosion inhibitor were also prepared and the effect of Ce(NO3)3 concentrations on the morphology and corrosion resistance of the coatings were examined. The surface chemistry and morphology of the hybrid sol-gel coatings were analyzed by Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The corrosion behavior of the coated aluminum alloy samples was evaluated by electrochemical impedance spectroscopy (EIS). Results revealed that good corrosion resistance of hybrid sol-gel coatings were prepared from hydrolysis and condensation reactions of GPTMS, TEOS and TPOZ precursors deposited on AA6111 aluminum alloy. When the coating doped with cerium nitrate, the properties were improved significantly. The hybrid sol-gel coatings containing lower concentration of cerium nitrate offer the best inhibition performance. A proper doping concentration of Ce(NO3)3 can effectively improve the corrosion resistance of the alloy, while an excessive concentration of Ce(NO3)3 would reduce the corrosion protection properties, which is associated with defective morphology and instability of the sol-gel coatings.

Keywords: AA6111, Ce(NO3)3, corrosion, hybrid sol-gel coatings

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Authors: Fetta Ait Ahsene-Aissat, Messaoud Hachemi, Yacine Moussaoui, Yacine Kerchiche

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Our study focuses on two important aspects, environmental by using a sub industrial product (FAD), by economic incorporation as an addition to Portland cement, thus improving resistance to compression and bending with different proportions ADF % up to 40 additions. We studied the effect of different substitutions 0%, 10%, 20%, and 40% of additions to the mechanical effect of the mortar. We obtained a compressive strength of 61 MPa at 90 days for the cement mixture porthland FAD-40% against a resistance of 58MPa for porthland cement without addition. The flexural strength also showed a marked increase in the cement substitution. We also monitored the behavior of the mixed ash-cement by XRD analysis and scanning electron microscopy (SEM).

Keywords: FAD, porthland, flexural strength, compressive strength, DRX

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Authors: Behrooz Ghasemi, Bahram Sharijian

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Al2O3/Mo nanocomposite powders were successfully synthesized by mechanical milling through mechanochemical reaction between MoO3 and Al. The structural evolutions of powder particles during mechanical milling were studied by X-ray diffractometry (XRD), energy dispersive X-ray spectroscopy(EDX) and scanning electron microscopy (SEM). Results show that Al2O3-Mo was completely obtained after 5 hr of milling. The crystallite sizes of Al2O3 and Mo after milling for 20 hr were about 45 nm and 23 nm, respectively. With longer milling time, the intensities of Al2O3 and Mo peaks decreased and became broad due to the decrease in crystallite size. Morphological features of powders were influenced by the milling time. The resulting Al2O3- Mo nanocomposite powder exhibited an average particle size of 200 nm after 20 hr of milling. Also nanocomposite powder after 10 hr milling had relatively equiaxed shape with uniformly distributed Mo phase in Al2O3 matrix.

Keywords: Al2O3/Mo, nanocomposites, mechanochemical, mechanical milling

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Authors: Yogita Patil-Sen

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

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

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Authors: Leila Samiee, Amir Yadegari, Saeedeh Tasharrofi

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In the work presented here, nitrogen-doped graphene materials were synthesized and used as metal-free electrocatalysts for oxygen reduction reaction (ORR) under alkaline conditions. Paraphenylenediamine was used as N precursor. The N-doped graphene was synthesized under hydrothermal treatment at 200°C. All the materials have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM) and X-ray photo-electron spectroscopy (XPS). Moreover, for electrochemical evaluation of samples, Rotating Disk electrode (RDE) and Cyclic Voltammetry techniques (CV) were employed. The resulting material exhibits an outstanding catalytic activity for the oxygen reduction reaction (ORR) as well as excellent resistance towards methanol crossover effects, indicating their promising potential as ORR electrocatalysts for alkaline fuel cells.

Keywords: alkaline fuel cell, graphene, metal-free catalyst, paraphenylen diamine

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Authors: F. A. Rodríguez-Prada, W Gutierrez, I. D. Mikhailov

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We study the spectral properties of one-electron non-uniform crater-shaped quantum dot whose thickness is increased linearly with different slopes in different radial directions between the central hole and the outer border and which is deposited over thin wetting layer in the presence of the external vertically directed magnetic field. We show that in the adiabatic limit, when the crater thickness is much smaller than its lateral dimension, the one-particle wave functions of the electron confined in such structure in the zero magnetic field case can be found exactly in an analytical form and they can be used subsequently as the base functions in framework of the exact diagonalization method to study the effect of the wetting layer and an external magnetic field applied along of the grown axis on energy levels of one-electron non-uniform quantum dot. It is shown that both the structural non-uniformity and the increase of the thickness of the wetting layer provide a quenching of the Aharonov-Bohm oscillations of the lower energy levels.

Keywords: electronic properties, quantum rings, volcano shaped, wetting layer

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Authors: Fernández-Brito David, Lopez-Medina Javier Alonso, Murillo-Bracamontes Eduardo Antonio, Palomino-Ovando Martha Alicia, Gervacio-Arciniega José Juan

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Magnetic Force Microscopy (MFM) is an Atomic Force Microscopy (AFM) technique that characterizes, at a nanometric scale, the magnetic properties of ferromagnetic materials. Conventional MFM works by scanning in two different AFM modes. The first one is tapping mode, in which the cantilever has short-range force interactions with the sample, with the purpose to obtain the topography. Then, the lift AFM mode starts, raising the cantilever to maintain a fixed distance between the tip and the surface of the sample, only interacting with the magnetic field forces of the sample, which are long-ranged. In recent years, there have been attempts to improve the MFM technique. Bimodal MFM was first theoretically developed and later experimentally proven. In bimodal MFM, the AFM internal piezoelectric is used to cause the cantilever oscillations in two resonance modes simultaneously, the first mode detects the topography, while the second is more sensitive to the magnetic forces between the tip and the sample. However, it has been proven that the cantilever vibrations induced by the internal AFM piezoelectric ceramic are not optimal, affecting the bimodal MFM characterizations. Moreover, the Secondary Resonance Magnetic Force Microscopy (SR-MFM) was developed. In this technique, a coil located below the sample generates an external magnetic field. This alternating magnetic field excites the cantilever at a second frequency to apply the Bimodal MFM mode. Nonetheless, for ferromagnetic materials with a low coercive field, the external field used in SR-MFM technique can modify the magnetic domains of the sample. In this work, a Hybrid Bimodal MFM (HB-MFM) technique is proposed. In HB-MFM, the bimodal MFM is used, but the first resonance frequency of the cantilever is induced by the magnetic field of the ferromagnetic sample due to its vibrations caused by a piezoelectric element placed under the sample. The advantages of this new technique are demonstrated through the preliminary results obtained by HB-MFM on a hard disk sample. Additionally, traditional two pass MFM and HB-MFM measurements were compared.

Keywords: magnetic force microscopy, atomic force microscopy, magnetism, bimodal MFM

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Authors: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: Sudkate Chaiyo, Weena Siangproh, Orawon Chailapakul, Kurt Kalcher

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In the present work, a simple and sensitive non-enzymatic electrochemical detection of glucose in disposable paper-based sensor was developed at ionic liquid/graphene/cobalt phthalocyanine composite (IL/G/CoPc) modified electrode. The morphology of the fabricated composite was characterized and confirmed by scanning electron microscopy and UV-Vis spectroscopy. The UV-Vis spectroscopy results confirmed that the G/CoPc composite formed via the strong π–π interaction between CoPc and G. Amperometric i-t technique was used for the determination of glucose. The response of glucose was linear over the concentration ranging from 10 µM to 1.5 mM. The response time of the sensor was found as 30 s with a limit of detection of 0.64 µM (S/N=3). The fabricated sensor also exhibited its good selectivity in the presence of common interfering species. In addition, the fabricated sensor exhibited its special advantages such as low working potential, good sensitivity along with good repeatability and reproducibility for the determination of glucose.

Keywords: glucose, paper-based sensor, ionic liquid/graphene/cobalt phthalocyanine composite, electrochemical detection

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Authors: Mirijam Vrabec, Marian Janak, Bojan Ambrozic, Angelja K. Surca, Nastja Rogan Smuc, Nina Zupancic, Saso Sturm

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Natural microdiamonds and moissanite (SiC) can form during the orogenic events under ultrahigh-pressure metamorphic conditions (UHP), when parts of Earth’s crust are subducted to extreme depths. So far, such processes were identified only in few places on the Earth, and therefore, represent unique opportunity to study the evolution of the Earth’s deep interior. An important discovery of microdiamonds and moissanite was reported from Pohorje, (Slovenia), where they occurred as single or polyphase inclusions in garnets. Metasedimentary rocks from Pohorje are predominantly gneisses representing parts of the Austroalpine metamorphic units of the Eastern Alps. During Cretaceous orogeny, (ca. 95–92 Ma) continental crustal rocks were deeply subducted to the mantle depths (below 100 km) and metamorphosed at pressures exceeding 3.5 GPa and temperatures between 800–850 °C. Microstructural and phase analysis of the inclusions as well as detailed elemental analysis of host garnets were carried out combining several analytical techniques: optical microscope in plane polarized transmitted light, electron probe microanalysis (EPMA) with wavelength-dispersive x-ray spectrometry (WDS) and field-emission scanning microscope (FEG-SEM) with energy-dispersive x-ray spectroscopy (EDS). Micro-Raman analysis revealed sharp, first order diamond bands sometimes accompanied by graphite bands implying that transformation of diamond back to graphite occurred. To study the chemical and crystallographic relationship between microdiamonds and co-inclusions, advanced techniques of transmission electron microscopy (TEM) were applied, which included high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), combined with EDS and electron energy-loss spectroscopy (EELS). To prepare electron transparent TEM lamellae selectively a dual-beam Focused Ion Beam/SEM (FIB/SEM) was employed. Detailed study of TEM lamellae, which was cross-sectioned from the highly faceted inclusion body located within the host garnet crystal matrix, revealed rich and rather complex internal structure. Namely, the negative crystal facets of the main inclusion body were typically decorated with up to 1 μm thick amorphous layer, reflecting the general garnet composition with slight variations in Fe/Ca content. Within these layers, ELNES analysis revealed the presence of a 28–30 nm thick layer of amorphous carbon. The very last section of this layer corresponds to composition of SiO2. Within the inclusion, besides diamond and moissanite alumosilicate mineral with pronounced layered structure, iron sulfides and chlorine were identified under TEM and CO2 and CH4 using Raman. Moissanite is found as single crystal or composed from numerous highly textured nano-crystals with the average size of 10 nm. Moissanite inclusions were found embedded inside the amorphous crust implying that moissanite crystalized well before the deposition of the amorphous layer. From the microstructural, crystallographic and chemical observations so far we can deduce, that polyphase inclusions in diamond bearing garnets from Pohorje most probably crystallized from reduced supercritical fluids. Based on layered interface structure of the host mineral multiphase process of crystallization is possible. The presence of microdiamonds and moissanite in rocks from Pohorje demonstrates that these parts of the Eastern Alps were subducted to extreme depths, and were subsequently exhumed back to the Earth's surface without complete breakdown of UHP mineral phases, allowing a rear and exceptional opportunity to study them in-situ.

Keywords: diamond, fluid inclusions, moissanite, TEM, UHP metamorphism.

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Authors: Osama Saber

Abstract:

Cyanate is one such anion which is produced during protein poisoning in the body and has been studied extensively in the field of biochemistry because of its toxicity. The present work aims at confinement and storage of cyanate in the nano scale. It was achieved through the intercalation of cyanate anions into nanolayerd structures of Ni-Al LDH. In addition, the effect of aging time on the intercalation of cyanate was clarified using X-ray diffraction and scanning electron microscopy. Furthermore, the effect of cations on the affinity towards the intercalation of cyanate anions inside LDH structure was studied by replacement of tetra-valent cations Ti4+ instead of the tri-vallent cations Al3+ during the preparation of LDH structure. X-ray diffraction patterns of the Ni-Ti LDH showed that the interlayer spacing was 0.73 nm. This spacing was smaller than that of Ni-Al LDH suggesting that the interlayered anions into Ni-Ti LDH are different from those into Ni-Al LDH. Thermal analyses (TG, DTG, and DTA) and Infra-red spectra revealed the presence of only cyanate anions into Ni-Ti LDH while, in the case of Ni-Al LDH, both cyanate and carbonate anions were observed. SEM images showed plate-like morphology for both Ni-Ti and Ni-Al LDHs although the shapes of their plates are not similar. Our results suggested that the LDH structures containing titanium cations have higher affinity for cyanate anions than those containing aluminum cations. Therefore, this choice for cyanate in the interlayered spacing widens the applicability to study the effect of the confinement on the toxicity of cyanate by bio researchers.

Keywords: nanolayered structures, Ni-Al LDH, Ni-Ti LDH, intercalation of cyanate anions, urea hydrolysis

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Authors: Monica Enculescu, A. Evanghelidis, I. Enculescu

Abstract:

Among the numerous methods for obtaining polymer nanofibers, the electrospinning technique distinguishes itself due to the more growing interest induced by its proved utility leading to developing and improving of the method and the appearance of novel materials. In particular, production of polymeric nanofibers in which different dopants are introduced was intensively studied in the last years because of the increased interest for the obtaining of functional electrospun nanofibers. Electrospinning is a facile method of obtaining polymer nanofibers with diameters from tens of nanometers to micrometrical sizes that are cheap, flexible, scalable, functional and biocompatible. Besides the multiple applications in medicine, polymeric nanofibers obtained by electrospinning permit manipulation of light at nanometric dimensions when doped with organic dyes or different nanoparticles. It is a simple technique that uses an electrical field to draw fine polymer nanofibers from solutions and does not require complicated devices or high temperatures. Different morphologies of the electrospun nanofibers can be obtained for the same polymeric host when different parameters of the electrospinning process are used. Consequently, we can obtain tuneable optical properties of the electrospun nanofibers (e.g. changing the wavelength of the emission peak) by varying the parameters of the fabrication method. We focus on obtaining doped polymer nanofibers with enhanced optical properties using the electrospinning technique. The aim of the paper is to produce dye-doped polymer nanofibers’ mats incorporating uniformly dispersed dyes. Transmission and fluorescence of the fibers will be evaluated by spectroscopy methods. The morphological properties of the electrospun dye-doped polymer fibers will be evaluated using scanning electron microscopy (SEM). We will tailor the luminescent properties of the material by doping the polymer (polyvinylpyrrolidone or polymethylmetacrilate) with different dyes (coumarins, rhodamines and sulforhodamines). The tailoring will be made taking into consideration the possibility of changing the luminescent properties of electrospun polymeric nanofibers that are doped with different dyes by using different parameters for the electrospinning technique (electric voltage, distance between electrodes, flow rate of the solution, etc.). Furthermore, we can evaluated the influence of the concentration of the dyes on the emissive properties of dye-doped polymer nanofibers using different concentrations. The advantages offered by the electrospinning technique when producing polymeric fibers are given by the simplicity of the method, the tunability of the morphology allowed by the possibility of controlling all the process parameters (temperature, viscosity of polymeric solution, applied voltage, distance between electrodes, etc.), and by the absence of necessity of using harsh and supplementary chemicals such as the ones used in the traditional nanofabrication techniques. Acknowledgments: The authors acknowledge the financial support received through IFA CEA Project No. C5-08/2016.

Keywords: electrospinning, luminescence, polymer nanofibers, scanning electron microscopy

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Authors: Venkataraman Sivasankar, Kiyoshi Omine, Hideaki Sano

Abstract:

The leaching of fluoride from Plaster Board Waste (PBW) is quite feasible in soil and water environments. The Ministry of Environment, Japan recommended the standard limit of 0.8 mgL⁻¹ or less for fluoride. Although the utilization of PBW as a substitute for cement is rather meritorious, its fluoride leaching behavior deteriorates the quality of soil and water and therefore envisaged as a demerit. In view of this fluoride leaching problem, the present research is focused on immobilizing fluoride in PBW. The immobilization experiments were conducted with four chemical systems operated by DAHP (diammonium hydrogen phosphate) and phosphoric acid carbonization of bamboo mass coupled with certain inorganic reactions using reagents such as calcium hydroxide, sodium hydroxide, and aqueous ammonia. The fluoride immobilization was determined after shaking the reactor contents including the plaster board waste for 24 h at 25˚C. In the DAHP system, the immobilization of fluoride was evident from the leaching of fluoride in the range 0.071-0.12 mgL⁻¹, 0.026-0.14 mgL⁻¹ and 0.068-0.12 mgL⁻¹ for the reaction temperatures at 30˚C, 50˚C, and 90˚C, respectively, with final pH of 6.8. The other chemical systems designated as PACCa, PACAm, and PACNa could immobilize fluoride in PBW, and the resulting solution was analyzed with the fluoride less than the Japanese environmental standard of 0.8 mgL⁻¹. In the case of PACAm and PACCa systems, the calcium concentration was found undetectable and witnessed the formation of phosphate compounds. The immobilization of fluoride was found inversely proportional to the increase in the volume of leaching solvent and dose of PBW. Characterization studies of PBW and the solid after fluoride immobilization was done using FTIR (Fourier transform infrared spectroscopy), Raman spectroscopy, FE-SEM ( Field Emission Scanning Electron Microscopy) with EDAX (Energy Dispersive Spectroscopy), XRD (X-ray diffraction), and XPS (X-ray photoelectron spectroscopy). The results revealed the formation of new calcium phosphate compounds such as apatite, monetite, and hydroxylapatite. The participation of such new compounds in fluoride immobilization seems indispensable through the exchange mechanism of hydroxyl and fluoride groups. Acknowledgment: First author thanks to Japanese Society for the Promotion of Science (JSPS) for the award of the fellowship (ID No. 16544).

Keywords: characterization, fluoride, immobilization, plaster board waste

Procedia PDF Downloads 157

Authors: Amel Asselah, Nadia Chabli, Imane Haddad

Abstract:

The adsorption of methylene blue and congo red dyes in an aqueous solution, on a food waste adsorbent: potato peel, and on a commercial adsorbent: activated carbon powder, was investigated using batch experiments. The objective of this study is the valorization of potato peel by its application in the elimination of these dyes. A comparison of the adsorption efficiency with a commercial adsorbent was carried out. Characterization of the potato peel adsorbent was performed by scanning electron microscopy coupled to energy-dispersive X-ray spectroscopy, Fourier transforms infrared spectroscopy, X-ray diffraction, and X-ray fluorescence. Various parameters were analyzed, in particular: the adsorbent mass, the initial dye concentration, the contact time, the pH, and the temperature. The results reveal that it is about 98% for methylene blue-potato peel, 84% for congo red-potato peel, 84% for methylene blue-activated carbon, and 66% for congo red-activated carbon. The kinetic data were modeled by different equations and revealed that the adsorption of textile dyes on adsorbents follows the model pseudo-second-order, and the particular extra diffusion governs the adsorption mechanism. It has been found that the adsorption process could be described by the Langmuir isotherm.

Keywords: bioadsorbent, waste valorization, adsorptio, textile dyes

Procedia PDF Downloads 91

Authors: M. Cabuk, M. Yavuz, T. A. Yesil, H. I. Unal

Abstract:

Electrorheological (ER) fluids are a class of smart materials exhibiting reversible changes in their rheological and mechanical properties under an applied electric field (E). ER fluids generally are composed of polarisable solid particles dispersed in non-conducting oil. ER fluids are fluids which exhibit. The resistance to motion of the ER fluid can be controlled by adjusting the applied E, due to their fast and reversible changes in their rheological properties presence of E. In this study, a series of chitosan/expanded perlite (CS/EP) composites with different chitosan mass fractions (10%, 20%, and 50%) was used. Characterizations of the composites were carried out by Fourier Transform Infrared (FTIR), X-ray diffraction (XRD) and Scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) techniques. Antisedimentation stability and dielectric properties of the composites were also determined. The effects of volume fraction, electric field strength, shear rate, shear stress, and temperature onto ER properties of the CS/EP composite particles dispersed in silicone oil (SO) were investigated in detail. Vibration damping behavior of the CS/EP composites were determined as a function of frequence, storage (Gʹ) and loss (Gʹ ʹ) moduli. It was observed that ER response of the CS/EP/SO ER fluids increased with increasing electric field strength and exhibited the typical shear thinning non-Newtonian viscoelastic behaviors with increasing shear rate. The maximum yield stress was obtained with 1250 Pa under E = 3 kV/mm. Further, the CS/EP/SO ER fluids were observed to sensitive to vibration control by showing reversible viscosity enhancements (Gʹ > Gʹ ʹ). Acknowledgements: The authors thank the TÜBİTAK (214Z199) for the financial support of this work.

Keywords: chitosan, electrorheology, perlite, vibration control

Procedia PDF Downloads 236

Authors: Abdelghani May

Abstract:

This paper reports on experimental investigations concerning the underlying reasons for the anisotropic behavior observed during the cyclic loading of AA2017 aluminum alloy. Initially, we quantified the evolution of fatigue damage resulting from controlled proportional cyclic loadings along the axial and shear directions. Our primary objective at this stage was to verify the anisotropic mechanical behavior recently observed. To accomplish this, we utilized various models of fatigue damage quantification and conducted a comparative study of the obtained results. Our analysis confirmed the anisotropic nature of the material under investigation. In the subsequent step, we performed microstructural investigations aimed at understanding the origins of the anisotropic mechanical behavior. To this end, we utilized scanning electron microscopy to examine the phases and precipitates in both the transversal and longitudinal sections. Our findings indicate that the structure and morphology of these entities are responsible for the anisotropic behavior observed in the aluminum alloy. Furthermore, results obtained from Kikuchi diagrams, pole figures, and inverse pole figures have corroborated these conclusions. These findings demonstrate significant differences in the crystallographic texture of the material.

Keywords: microstructural investigation, fatigue damage quantification, anisotropic behavior, AA2017 aluminum alloy, cyclic loading, crystallographic texture, scanning electron microscopy

Procedia PDF Downloads 76

Authors: C. D. Gomez-Esparza, Z. V. Hernandez-Castro, C. A. Rodriguez-Gonzalez, R. Martinez-Sanchez, A. Duarte-Moller

Abstract:

Recently, the high entropy alloys (HEA) are the focus of attention in metallurgical and materials science due to their desirable and superior properties in comparison to conventional alloys. The HEA field has promoted the exploration of several compositions including the addition of non-metallic elements like carbon, which in traditional metallurgy is mainly used in the steel industry. The aim of this work was the synthesis of equiatomic FeCrNiMnTi high entropy alloys, with minor carbon content, by mechanical alloying and sintering. The effect of the addition of carbon nanotubes and graphite were evaluated by X-ray diffraction, scanning electron microscopy, and microhardness test. The structural and microstructural characteristics of the equiatomic alloys, as well as their hardness were compared with those of an austenitic AISI 321 stainless steel processed under the same conditions. The results showed that porosity in bulk samples decreases with carbon nanotubes addition, while the equiatomic composition favors the formation of titanium carbide and increased the AISI 321 hardness more than three times.

Keywords: carbon nanotubes, graphite, high entropy alloys, mechanical alloying

Procedia PDF Downloads 198

Authors: Azadeh Farzaneh, Mohammad Reza Abdi, A. Quaranta, Matteo Dalla Palma, Seyedshahram Mortazavi

Abstract:

We report on the synthesis of cesium-iodide nanoparticles using sol-gel technique. The structural properties of CsI nanoparticles were characterized by X-ray diffraction and Scanning Electron Microscope (SEM) Also, optical properties were followed by optical absorption and UV–vis fluorescence. Intense photoluminescence is also observed, with some spectral tuning possible with ripening time getting a range of emission photon wavelength approximately from 366 to 350 nm. The size effect on CsI luminescence leads to an increase in scintillation light yield, a redshift of the emission bands of the on_center and off_center self_trapped excitons (STEs) and an increase in the contribution of the off_center STEs to the net intrinsic emission yield. The energy transfer from the matrix to CsI nanoparticles is a key characteristic for scintillation detectors. So the scintillation spectra to alpha particles of sample were monitored.

Keywords: nanoparticles, luminescence, sol gel, scintillator

Procedia PDF Downloads 599

Authors: D. V. S. Praneeth, V. R. Sankar Cheela, Brajesh Dubey

Abstract:

Coal Combustion (CC) residues are the major by-products from thermal power plants. The disposal of ash on to land creates havoc to environment and humans. The leaching of the constituent elements pollutes ground water. Beneficiary use of coal combustion residues in structural components is being investigated as a part of this study. This application reduces stress on the convention materials in the construction industry. The present study involves determination of leaching parameters of the CC residues. Batch and column studies are performed based on Leaching Environmental Assessment Framework (LEAF) protocol. The column studies are conducted to simulate the real time percolation conditions in the field. The structural and environmental studies are performed to determine the usability of CC residues as bricks. The physical, chemical, geo environmental and mechanical properties of the alternate materials are investigated. Scanning electron microscopy (SEM), X-Ray Diffraction analysis (XRD), X-ray fluorescence (XRF) and Energy Dispersive X-ray Spectroscopy tests were conducted to determine the characteristics of CC residue ash and bricks.

Keywords: coal combustion residues, LEAF, leaching, SEM

Procedia PDF Downloads 314

Authors: Omaima G. Allam, O. A. Hakeim, K. Haggag, N. S. Elshemy

Abstract:

In the midst of the two decades the use of microwave dielectric warming in the field of science has transformed into a powerful methodology to redesign compound procedures. The potential benefit of the application of these modern methods of treatment emphasize so as to reach to optimum treatment conditions and the best results, especially hydrophobicity, moisture content and increase dyeing processing while maintaining the physical and chemical properties of each textile. Moreover, polyester fibres are sometimes spun together with natural fibres to produce a cloth with blended properties. So that at the present task, the polyester/viscose mix fabrics (60 /40) were pretreated with 4 g/l of KOH for 2 min in microwave irradiation with a liquor ratio 1:25. Subsequently fabrics were inundated with different concentrations of sericin (10, 30, 50 g/l). Treated fabrics were coloured with the commercial dyes samples: Reactive Red 84(Dye 1). C. I. Acid Blue 203(Dye 2) and C.I. Reactive violet 5 (Dye 3). Colour value was specified as well as fastness properties. Likewise, the physical properties of untreated and treated fabrics such as moisture content %, tensile strength, elongation % and were evaluated. The untreated and treated fabrics are described by infrared spectroscopy (FTIR) and scanning electron microscopy.

Keywords: polyester viscose blends fabric, sericin, dyes, colour value

Procedia PDF Downloads 239