Search results for: scanning electron microscope (SEM)

Authors: Kshanaprava Dhalsamant, Punyadarshini P. Tripathy, Shanker L. Shrivastava

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With present high global population, the need for rising food usage by minimizing food wastage and investment is highly necessary to achieve food security. The purpose of this study is to enlighten the effect of pre-drying treatment on rehydration, color, texture, nanohardness, microstructure and surface morphology of solar dried potato samples dried in the mixed-mode solar dryer. Locally bought potatoes were cleaned and cut into cylindrical pieces and pretreated with sodium metabisulfite (0.5%) for 10 min before placing them in natural convection solar dryer designed and developed in Indian Institute of Technology Kharagpur, India. Advanced quality characteristics were studied using Atomic Force Microscope (AFM), Scanning Electron Microscopy (SEM) and nanoindentation method, along with color, texture and water activity. The rehydration indices of solar dried potatoes were significantly biased by pretreatment followed by rehydration temperature. A lower redness index (a*) with a higher value of yellowness index (b*), chroma (C*) and hue angle (h*) were obtained for pretreated samples. Also, the average nanohardness (H) of untreated samples exhibited substantial lower value (18.46%) compared to pretreated samples. Additionally, a creep displacement of 43.27 nm during 20 s dwell time under constant load of 200

Keywords: pretreatment, nanohardness, microstructure, surface morphology

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Authors: Maha Al-Ali, Selvakannan Periasamy, Rajarathinam Parthasarathy

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Drying temperature is an important factor impacting the physicochemical properties of the dried materials, particularly the pharmaceutical powders. Drying of pharmaceuticals by using microwave radiation is very limited, and the available information about the interaction between the electromagnetic radiations and the pharmaceutical material is still scarce. Therefore, microwave drying process is employed in this work to dry the wet (moisturised) granules of the formulated naproxen-sodium drug. This study aims to investigate the influences of the microwave radiation temperatures on the moisture removal, the crystalline structure, the size and morphology of the dried naproxen-sodium particles, and identify any potential changes in the chemical groups of the drug. In this work, newly formulated naproxen-sodium is prepared and moisturized by wet granulation process and hence dried by using microwave radiation at different temperatures. Moisture analyzer, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and scanning electron microscope are used to characterise the non-moisturised powder (reference powder), the moisturised granules, and the dried particles. The results show that microwave drying of naproxen-sodium at high drying temperature is more efficient than that at low temperatures in terms of the moisture removal. Although there is no significant change in the chemical structure of the dried particles, the particle size, crystallinity and morphology are relatively changed with changing of heating temperature.

Keywords: heating temperature, microwave drying, naproxen-sodium, particle size

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy (FTIR), micro-Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence Spectroscopy (PL) and Field Effect Scanning electron microscopy (FESEM)

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Authors: JongWon Han, NoHoon Kim, HyoIk Ahn, HaeWoo Lee

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In this study, shielded metal arc welding was performed as a function of Nb content at 2.24 wt%, 3.25 wt%, and 4.26 wt%. The microstructure was observed using scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and showed the development of a columnar dendrite structure in the specimen having the least Nb content. From the hardness test, the hardness value was confirmed to reduce with decreasing Nb content. From electron backscatter diffraction (EBSD) analysis, the largest grain size was found in the specimen with Nb content of 2.24 wt%. The potentiodynamic polarization test was carried out to determine the pitting corrosion resistance; there was no significant difference in the pitting corrosion resistance with increasing Nb content. To evaluate the degree of sensitization to intergranular corrosion, the Double Loop Electrochemical Potentiodynamic Reactivation(DL-EPR test) was conducted. A similar degree of sensitization was found in two specimens except with a Nb content of 2.24 wt%, while a relatively high degree of sensitization was found in the specimen with a Nb content of 2.24 wt%.

Keywords: inconel 625, Nb content, potentiodynamic test, DL-EPR test

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Authors: Dahi Ghareab Abdelsalam Ibrahim

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Scanning interferometry is commonly used for measuring the three-dimensional profiling of surfaces. Here, we used a scanning stage calibrated with standard gauge blocks to measure a standard step height of 200μm. The stage measures precisely the envelope of interference at the platen and at the surface of the step height. From the difference between the two envelopes, we measured the step height of the sample. Experimental measurements show that the measured value matches well with the nominal value of the step height. A light beam of 532nm from a Tungsten Lamp is collimated and incident on the interferometer. By scanning, two envelopes were produced. The envelope at the platen surface and the envelope at the object surface were determined precisely by a written program code, and then the difference between them was measured from the calibrated scanning stage. The difference was estimated to be in the range of 198 ± 2 μm.

Keywords: optical metrology, digital holography, interferometry, phase unwrapping

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Authors: Mahnoosh Aliahmadi, Akbar Esmaeili

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This study synthesized new modified imaging nanocapsules (NCs) of gallium@deferoxamine/folic acid/chitosan/polyaniline/polyvinyl alcohol (Ga@DFA/FA/CS/PANI/PVA) containing Morus nigra extract by selenium nanoparticles prepared from Lactobacillus acidophilus. Se nanoparticles were then deposited on (Ga@DFA/FA/CS/PANI/PVA) using the impregnation method. The modified contrast agents were mixed with M. nigra extract, and their antibacterial activities were investigated by applying them to L929 cell lines. The influence of variable factors including surfactant, solvent, aqueous phase, pH, buffer, minimum Inhibitory concentration (MIC), minimum bactericidal concentration (MBC), cytotoxicity on cancer cells, antibiotic, antibiogram, release and loading, stirring effect, the concentration of nanoparticle, olive oil, and thermotical methods was investigated. The structure and morphology of the synthesized contrast agents were characterized by zeta potential sizer analysis (ZPS), X-Ray diffraction (XRD), Fourier-transform infrared (FT-IR), and energy-dispersive X-ray (EDX), ultraviolet-visible (UV-Vis) spectra, and scanning electron microscope (SEM). The experimental section was conducted and monitored by response surface methods (RSM) and MTT conversion assay. Antibiogram testing of NCs on Pseudomonas aeruginosa bacteria was successful, and the MIC=2 factor was obtained with a less harmful effect.

Keywords: imaging contrast agent, nanoparticles, response surface method, Lactobacillus acidophilus, selenium

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Authors: Norul Hisham Hamid, Amir Affan, Ummi Hani Abdullah, Paridah Md. Tahir, Khairul Akmal Azhar, Rahmat Nawai, W. B. H. Wan Sulwani Izzati

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The dimensional stability and static bending properties of epoxy composite reinforced with amorphous and crystalline silica were investigated. The amorphous and crystalline silica was obtained by the precipitation method from carbonisation process of the rice husk at a temperature of 600 °C and 1000 °C for 7 hours respectively. The epoxy resin was mixed with 5%, 10% and 15% concentrations of amorphous and crystalline silica. The mixture was stirred for 10 minutes and cured at 28 °C for 72 hours and oven dried at 80 °C for 72 hours. The scanning electron microscope image showed the silica sized of 10-30nm was obtained. The water absorption and thickness swelling of epoxy/amorphous silica composite was not significantly different with silica concentration ranged from 0.08% to 0.09% and 0.17% to 0.20% respectively. The maximum modulus of rupture (85 MPa) and modulus of elasticity (3284 MPa) were achieved for 10% silica concentration. For epoxy/crystalline silica composite; the water absorption and thickness swelling were also not significantly different with silica concentration, ranged from 0.08% to 0.11% and 0.16% to 0.18% respectively. The maximum modulus of rupture (47.9 MPa) and modulus of elasticity (2760 MPa) were achieved for 10% silica concentration. Overall, the water absorption and thickness swelling were almost identical for epoxy composite made from either amorphous or crystalline silica. The epoxy composite made from amorphous silica was stronger than crystalline silica.

Keywords: epoxy, composite, dimensional stability, static bending, silica

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Authors: Raghvendra Singh Yadav, Ivo Kuritka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda, Milan Masar

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The elastomer nanocomposites were synthesized by solution mixing method with an elastomer as a matrix and in situ thermally reduced graphene oxide (RGO) and spinel ferrite NiFe₂O₄ nanoparticles as filler. Spinel ferrite NiFe₂O₄ nanoparticles were prepared by the starch-assisted sol-gel auto-combustion method. The influence of filler on the microstructure, morphology, dielectric, electrical and magnetic properties of Reduced Graphene Oxide-Nickel Ferrite-Elastomer nanocomposite was characterized by X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X-ray photoelectron spectroscopy, the Dielectric Impedance analyzer, and vibrating sample magnetometer. Scanning electron microscopy study revealed that the fillers were incorporated in elastomer matrix homogeneously. The dielectric constant and dielectric tangent loss of nanocomposites was decreased with the increase of frequency, whereas, the dielectric constant increases with the addition of filler. Further, AC conductivity was increased with the increase of frequency and addition of fillers. Furthermore, the prepared nanocomposites exhibited ferromagnetic behavior. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: polymer-matrix composites, nanoparticles as filler, dielectric property, magnetic property

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Authors: S. M. Giripunje, Shikha Jindal

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

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

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Authors: Temesgen Geremew

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ZnS/glass and CdS/glass single layers and ZnS/CdS and CdS/ZnS heterojunction thin films were deposited by the chemical bath deposition method using zinc acetate and cadmium acetate as the metal ion sources and thioacetamide as a nonmetallic ion source in acidic medium. Na2EDTA was used as a complexing agent to control the free cation concentration. +e single layer and heterojunction thin films were characterized with X-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive X-ray (EDX), and a UV-VIS spectrometer. +e XRD patterns of the CdS/glass thin film deposited on the soda lime glass substrate crystalized in the cubic structure with a single peak along the (111) plane. +e ZnS/CdS heterojunction and ZnS/glass single layer thin films were crystalized in the hexagonal ZnS structure. +e CdS/ZnS heterojunction thin film is nearly amorphous.The optical analysis results confirmed single band gap values of 2.75 eV and 2.5 eV for ZnS/CdS and CdS/ZnS heterojunction thin films, respectively. +e CdS/glass and CdS/ZnS thin films have more imaginary dielectric components than the real part. The optical conductivity of the single layer and heterojunction films is in the order of 1015 1/s. +e optical study also confirmed refractive index values between 2 and 2.7 for ZnS/glass, ZnS/CdS, and CdS/ZnS thin films for incident photon energies between 1.2 eV and 3.8 eV. +e surface morphology studies revealed compacted spherical grains covering the substrate surfaces with few cracks on ZnS/glass, ZnS/CdS, and CdS/glass and voids on CdS/ZnS thin films. +e EDX result confirmed nearly 1 :1 metallic to nonmetallic ion ratio in the single-layered thin films and the dominance of Zn ion over Cd ion in both ZnS/CdS and CdS/ZnS heterojunction thin films.

Keywords: SERS, sensor, Hg2+, water detection, polythiophene

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Authors: Hamza Shams, Sajid Saleem, Bilal A. Siddiqui

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This paper investigates the coefficient of friction at nano-levels of commercially available superhydrophobic/oleophobic coatings when applied over 316L SS. 316L Stainless Steel or Marine Stainless Steel has been selected for its widespread uses in structures, marine and biomedical applications. The coatings were investigated in harsh sand-storm and sea water environments. The particle size of the sand during the procedure was carefully selected to simulate sand-storm conditions. Sand speed during the procedure was carefully modulated to simulate actual wind speed during a sand-storm. Sample preparation was carried out using prescribed methodology by the coating manufacturer. The coating’s adhesion and thickness was verified before and after the experiment with the use of Scanning Electron Microscopy (SEM). The value for nano-level coefficient of friction has been determined using Lateral Force Microscopy (LFM). The analysis has been used to formulate a value of friction coefficient which in turn is associative of the amount of wear the coating can bear before the exposure of the base substrate to the harsh environment. The analysis aims to validate the coefficient of friction value as marketed by the coating manufacturers and more importantly test the coating in real-life applications to justify its use. It is expected that the coating would resist exposure to the harsh environment for a considerable amount of time. Further, it would prevent the sample from getting corroded in the process.

Keywords: 316L SS, scanning electron microscopy, lateral force microscopy, marine stainless steel, oleophobic coating, superhydrophobic coating

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Authors: Tadahiro Wada, Hiroyuki Hanyu

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In this study, to clarify the effectiveness of an aluminum/chromium/tungsten-based-coated tool for cutting sintered steel, tool wear was experimentally investigated. The sintered steel was turned with the (Al60,Cr25,W15)N-, (Al60,Cr25,W15)(C,N)- and (Al64,Cr28,W8)(C,N)-coated cemented carbide tools according to the physical vapor deposition (PVD) method. Moreover, the tool wear of the aluminum/chromium/tungsten-based-coated item was compared with that of the (Al,Cr)N coated tool. Furthermore, to clarify the tool wear mechanism of the aluminum/chromium/tungsten-coating film for cutting sintered steel, Scanning Electron Microscope observation and Energy Dispersive x-ray Spectroscopy mapping analysis were conducted on the abraded surface. The following results were obtained: (1) The wear progress of the (Al64,Cr28,W8)(C,N)-coated tool was the slowest among that of the five coated tools. (2) Adding carbon (C) to the aluminum/chromium/tungsten-based-coating film was effective for improving the wear-resistance. (3) The main wear mechanism of the (Al60,Cr25,W15)N-, the (Al60,Cr25,W15)(C,N)- and the (Al64,Cr28,W8)(C,N)-coating films was abrasive wear.

Keywords: cutting, physical vapor deposition coating method, tool wear, tool wear mechanism, (Al, Cr, W)N-coating film, (Al, Cr, W)(C, N)-coating film, sintered steel

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Authors: Haiming Wen, Isabella J. Van Rooyen

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Tristructural isotropic (TRISO)-coated fuel particles are designed as nuclear fuel for high-temperature gas reactors. TRISO coating consists of layers of carbon buffer, inner pyrolytic carbon (IPyC), SiC, and outer pyrolytic carbon. The TRISO coating, especially the SiC layer, acts as a containment system for fission products produced in the kernel. However, release of certain metallic fission products across intact TRISO coatings has been observed for decades. Despite numerous studies, mechanisms by which fission products migrate across the coating layers remain poorly understood. In this study, scanning transmission electron microscopy (STEM), energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS) were used to examine the distribution, composition and structure of fission products in a TRISO coated particle neutron irradiated to 3.6 x 1021 n/cm² fast fluence at 1040 ⁰C. Precession electron diffraction was used to investigate characters of grain boundaries where specific fission product precipitates are located. The retention fraction of 110mAg in the investigated TRISO particle was estimated to be 0.19. A high density of nanoscale fission product precipitates was observed in the SiC layer close to the SiC-IPyC interface, most of which are rich in Pd, while Ag was not identified. Some Pd-rich precipitates contain U. Precipitates tend to have complex structure and composition. Although a precipitate appears to have uniform contrast in STEM, EDS indicated that there may be composition variations throughout the precipitate, and HRTEM suggested that the precipitate may have several parts different in crystal structure or orientation. Attempts were made to measure charge states of precipitates using EELS and study their possible effect on precipitate transport.

Keywords: TRISO particle, fission product, nuclear fuel, electron microscopy, neutron irradiation

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Authors: Gabi N. Nehme, Saeed Ghalambor

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The use of titanium fluoride and iron fluoride (TiF3/FeF3) catalysts in combination with polutetrafluoroethylene (PTFE) in plain zinc dialkyldithiophosphate (ZDDP) oil is important for the study of engine tribocomponents and is increasingly a strategy to improve the formation of tribofilm and to provide low friction and excellent wear protection in reduced phosphorus plain ZDDP oil. The influence of surface roughness and the concentration of TiF3/FeF3/PTFE were investigated using bearing steel samples dipped in lubricant solution @100°C for two different heating time durations. This paper addresses the effects of water drop contact angle using different surface finishes after treating them with different lubricant combination. The calculated water drop contact angles were analyzed using Design of Experiment software (DOE) and it was determined that a 0.05 μm Ra surface roughness would provide an excellent TiF3/FeF3/PTFE coating for antiwear resistance as reflected in the scanning electron microscopy (SEM) images and the tribological testing under extreme pressure conditions. Both friction and wear performance depend greatly on the PTFE/and catalysts in plain ZDDP oil with 0.05% phosphorous and on the surface finish of bearing steel. The friction and wear reducing effects, which was observed in the tribological tests, indicated a better micro lubrication effect of the 0.05 μm Ra surface roughness treated at 100°C for 24 hours when compared to the 0.1 μm Ra surface roughness with the same treatment.

Keywords: scanning electron microscopy, ZDDP, catalysts, PTFE, friction, wear

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Authors: Loai Ben Naji, Osama M. Ibrahim, Khaled J. Al-Fadhalah

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The objective of this paper is to investigate the formation and adhesion of a protective aluminum-oxide (Al₂O₃, alumina) layer on the surface of Iron-Chromium-Aluminum Alloy (Fe-Cr-Al) sintered-metal-fibers. The oxide-scale layer was developed via multi-stage thermal oxidation at 930 ^oC for 1 hour, followed by 1 hour at 960 ^oC, and finally at 990 ^oC for 2 hours. Scanning Electron Microscope (SEM) images show that the multi-stage thermal oxidation resulted in the formation of predominantly Al₂O₃ platelets-like and whiskers. SEM images also reveal non-uniform oxide-scale growth on the surface of the fibers. Furthermore, peeling/spalling of the alumina protective layer occurred after minimum handling, which indicates weak adhesion forces between the protective layer and the base metal alloy.  Energy Dispersive Spectroscopy (EDS) analysis of the heat-treated Fe-Cr-Al sintered-metal-fibers confirmed the high aluminum content on the surface of the protective layer, and the low aluminum content on the exposed base metal alloy surface. In conclusion, the failure of the oxide-scale protective layer exposes the base metal alloy to further oxidation, and the fragile non-uniform oxide-scale is not suitable as a support for catalysts.

Keywords: high-temperature oxidation, iron-chromium-aluminum alloy, alumina protective layer, sintered-metal-fibers

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Authors: Haolun Sun, Ping Wang, Mei Wu, Meng Zhang, Bin Hou, Ling Yang, Xiaohua Ma, Yue Hao

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Gallium nitride (GaN) is an attractive material for next-generation power devices. It is noted that the performance of GaN-based high electron mobility transistors (HEMTs) is always limited by the self-heating effect. In response to the problem, integrating devices with polycrystalline diamond (PCD) has been demonstrated to be an efficient way to alleviate the self-heating issue of the GaN-based HEMTs. Among all the heat-spreading schemes, using PCD to cap the epitaxial layer before the HEMTs process is one of the most effective schemes. Now, the mainstream method of fabricating the PCD-capped HEMTs is to deposit the diamond heat-spreading layer on the AlGaN surface, which is covered by a thin nucleation dielectric/passivation layer. To achieve the pattern etching of the diamond heat spreader and device preparation, we selected SiN as the hard mask for diamond etching, which was deposited by plasma-enhanced chemical vapor deposition (PECVD). The conventional diamond etching method first uses F-based etching to remove the SiN from the special window region, followed by using O₂/Ar plasma to etch the diamond. However, the results of the scanning electron microscope (SEM) and focused ion beam microscopy (FIB) show that there are lots of diamond pillars on the etched diamond surface. Through our study, we found that it was caused by the high roughness of the diamond surface and the existence of the overlap between the diamond grains, which makes the etching of the SiN hard mask insufficient and leaves micro-masks on the diamond surface. Thus, a cyclic etching method was proposed to solve the problem of the residual SiN, which was left in the F-based etching. We used F-based etching during the first step to remove the SiN hard mask in the specific region; then, the O₂/Ar plasma was introduced to etch the diamond in the corresponding region. These two etching steps were set as one cycle. After the first cycle, we further used cyclic etching to clear the pillars, in which the F-based etching was used to remove the residual SiN, and then the O₂/Ar plasma was used to etch the diamond. Whether to take the next cyclic etching depends on whether there are still SiN micro-masks left. By using this method, we eventually achieved the self-terminated etching of the diamond and the smooth surface after the etching. These results demonstrate that the cyclic etching method can be successfully applied to the integrated preparation of polycrystalline diamond thin films and GaN HEMTs.

Keywords: AlGaN/GaN heterojunction, O₂/Ar plasma, cyclic etching, polycrystalline diamond

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Authors: I. Shuro

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The crystal structure of Tin Sulfide prepared by certain chemical methods is investigated using High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), and X-ray diffraction (XRD) methods. An anomalous HRTEM Fast Fourier Transform (FFT) exhibited a central scatter of diffraction spots, which is surrounded by secondary clusters of spots arranged in a hexagonal pattern around the central cluster was observed. FFT analysis has revealed a long lattice parameter and mostly viewed along a hexagonal axis where there many columns of atoms slightly displaced from one another. This FFT analysis has revealed that the metal sulfide has a long-range order interwoven chain of atoms in its crystal structure. The observed crystalline structure is inconsistent with commonly observed FFT patterns of chemically synthesized Tin Sulfide nanocrystals and thin films. SEM analysis showed the morphology of a myriad of multi-shaped crystals ranging from hexagonal, cubic, and spherical micro to nanostructured crystals. This study also investigates the presence of quasi-crystals as reflected by the presence of mixed local symmetries.

Keywords: fast fourier transform, high resolution transmission electron microscopy, tin sulfide, crystalline structure

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Authors: Ainouna Bouziane

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The ability of Electron Tomography to recover the 3D structure of catalysts, with spatial resolution in the subnanometer scale, has been widely explored and reviewed in the last decades. A variety of experimental techniques, based either on Transmission Electron Microscopy (TEM) or Scanning Transmission Electron Microscopy (STEM) have been used to reveal different features of nanostructured catalysts in 3D, but High Angle Annular Dark Field imaging in STEM mode (HAADF-STEM) stands out as the most frequently used, given its chemical sensitivity and avoidance of imaging artifacts related to diffraction phenomena when dealing with crystalline materials. In this regard, our group has developed a methodology that combines image denoising by undecimated wavelet transforms (UWT) with automated, advanced segmentation procedures and parameter selection methods using CS-TVM (Compressed Sensing-total variation minimization) algorithms to reveal more reliable quantitative information out of the 3D characterization studies. However, evaluating the accuracy of the magnitudes estimated from the segmented volumes is also an important issue that has not been properly addressed yet, because a perfectly known reference is needed. The problem particularly complicates in the case of multicomponent material systems. To tackle this key question, we have developed a methodology that incorporates volume reconstruction/segmentation methods. In particular, we have established an approach to evaluate, in quantitative terms, the accuracy of TVM reconstructions, which considers the influence of relevant experimental parameters like the range of tilt angles, image noise level or object orientation. The approach is based on the analysis of material-realistic, 3D phantoms, which include the most relevant features of the system under analysis.

Keywords: electron tomography, supported catalysts, nanometrology, error assessment

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Authors: Andrea Alfaro Barajas, Arturo I. Martinez

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3D photothermal structure of carbon was synthesized using PET bottles waste and sodium chloride through controlled carbonization. Characterization techniques such as X-ray photoelectron spectroscopy, X-ray diffraction, BET, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, spectrophotometry, and mechanical compression were carried out. The carbon showed physical integrity > 90%, an absorbance > 90% between 300-1000nm of the solar spectrum, and a high specific surface area from 450 to 620 m2/g. The X-ray was employed to examine the phase structure; the obtained pattern shows an amorphous material. A higher intensity of band D with respect to band G was confirmed by Raman Spectroscopy. C-OH, COOH, C-O, and C-C bonds were obtained from the deconvolution of the high-resolution C1s orbital. Macropores of 160 to 180µm and micropores of 0.5 to 2nm were observed by SEM and TEM images, respectively. Such combined characteristics of carbon confer efficient evaporation of water under 1 sun irradiation > 60%.

Keywords: solar-absorber, carbon, water-evaporation, interfacial

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Authors: Ali Abdelnabi, Nermeen Hamza

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Coral calcium is a boasting natural product and dietary supplement which is considered a source of alkaline calcium carbonate, this study is a comparative study, comparing the remineralization effect of the new product of coral calcium with that of nano-hydroxyapatite. Methodology: a total of 35 extracted molars were collected, examined and sectioned to obtain 70 sound enamel discs, all discs were numbered and examined by scanning electron microscope coupled with Energy Dispersive Analysis of X-rays(EDAX) for mineral content, subjected to artificial caries, and mineral content was re-measured, discs were divided into seven groups according to the remineralizing agent used, where groups 1 to 3 used 10%, 20%, 30% nanohydroxyapatite gel respectively, groups 4 to 6 used 10%, 20%, 30% coral calcium gel and group 7 with no remineralizing agent (control group). All groups were re-examined by EDAX after remineralization; data were calculated and tabulated. Results: All groups showed a statistically significant drop in calcium level after artificial caries; all groups showed a statistically significant rise in calcium content after remineralization except for the control group; groups 1 and 5 showed the highest increase in calcium level after remineralization. Conclusion: coral calcium can be considered a comparative product to nano-hydroxyapatite regarding the remineralization of enamel initial carious lesions.

Keywords: artificial caries, coral calcium, nanohydroxyapatite, re-mineralization

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Authors: Mohamad Abdelfattah Ibrahim Elghrbawy

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This work deals to evaluate barium sulfate (BS) before and after its surface modification as reinforcing filler for rubber. Barium sulfate was surface-modified using polymethacrylic acid (PMAA), the monolayer surface coverage of barium sulfate by polymethacrylic acid molecules occurred at 5.4x10-6 mol/g adsorbed amount. This amount was sufficient to reduce the sediment volume from 2.65 to 2.55 cm3/gm. Natural rubber (NR) was compounded with different concentrations of barium sulfate. The rheological characteristics of NR mixes were measured using a Monsanto Oscillating Disk Rheometer. The compounded NR was vulcanized at 142°C, and the physico-mechanical properties were tested according to the standard methods. The rheological data show that the minimum torque decreases while the maximum torque increases as the barium sulfate content increase. The physico-mechanical properties of NR vulcanizates were improved up to 50 phr/ barium sulfate loading. On the other hand, styrene–butadiene rubber (SBR) and nitrile–butadiene rubber (NBR) rubbers compounded with 50 phr/barium sulfate had good rheological and mechanical properties. Scanning electron microscope studies show surface homogeneity of rubber samples as a result of good dispersion of surface modified barium sulfate in the rubber matrix. The NR, SBR and NBR vulcanizates keep their values of mechanical properties after subjected to thermal oxidative aging at 90°C for 7 days.

Keywords: barium sulfate, natural rubber (nr), nitrile–butadiene rubber (nbr), polymethacrylic acid (pmaa), styrene–butadiene rubber (sbr), surface modification

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Authors: Nilay K. Doshi

Abstract:

A theoretical probe describing the excited energy states of the electron density surrounding a nanoparticle (NP) is presented. An electromagnetic (EM) wave interacts with a NP much smaller than the incident wavelength. The plasmon that oscillates locally around the NP comprises of excited conduction electrons. The system is based on the Jellium model of a cluster of metal atoms. Hohenberg-Kohn (HK) equations and the variational Kohn-Sham (SK) scheme have been used to obtain the NP electron density in the ground state. Furthermore, a time-dependent density functional (TDDFT) theory is used to treat the excited states in a density functional theory (DFT) framework. The non-interacting fermionic kinetic energy is shown to be a functional of the electron density. The time dependent potential is written as the sum of the nucleic potential and the incoming EM field. This view of the quantum oscillation of the electron density is a part of the localized surface plasmon resonance.

Keywords: electron density, energy, electromagnetic, DFT, TDDFT, plasmon, resonance

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Authors: Ahmed Shariful Alam, Abu Hena M. Mustafa Kamal, M. Abdul Rahman, M. Nasmus Sakib Khan Shabbir, Atiqul Islam

Abstract:

According to the rules of quantum mechanics there is a non-vanishing probability of for an electron to tunnel through a thin insulating barrier or a thin capacitor which is not possible according to the laws of classical physics. Tunneling of electron through a thin insulating barrier or tunnel junction is a random event and the magnitude of current flowing due to the tunneling of electron is very low. As the current flowing through a Single Electron Transistor (SET) is the result of electron tunneling through tunnel junctions of its source and drain the supply voltage requirement is also very low. As a result, the power consumption across a Single Electron Transistor is ultra-low in comparison to that of a MOSFET. In this paper simulations have been done with PSPICE for an inverter built with both SETs and MOSFETs. 35mV supply voltage was used for a SET built inverter circuit and the supply voltage used for a CMOS inverter was 3.5V.

Keywords: ITRS, enhancement type MOSFET, island, DC analysis, transient analysis, power consumption, background charge co-tunneling

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Authors: Rudra Vaghela, P. K. Kulkarni

Abstract:

The aim of the present research was to develop oral Amphotericin B (AmB) nanocrystals (Nc) grafted with suitable ligand in order to enhance drug transport across the intestinal epithelial barrier and subsequently, active uptake by macrophages. AmB Nc were prepared by liquid anti-solvent precipitation technique (LAS). Poloxamer 188 was used to stabilize the prepared AmB Nc and grafted with mannose for actively targeting M cells in Peyer’s patches. To prevent shedding of the stabilizer and ligand, N,N’-Dicyclohexylcarbodiimide (DCC) was used as a cross-linker. The prepared AmB Nc were characterized for particle size, PDI, zeta potential, X-ray diffraction (XRD) and surface morphology using scanning electron microscope (SEM) and evaluated for drug content, in vitro drug release and cell uptake studies using caco-2 cells. The particle size of stabilized AmB Nc grafted with WGA was in the range of 287-417 nm with negative zeta potential between -18 to -25 mV. XRD studies revealed crystalline nature of AmB Nc. SEM studies revealed that ungrafted AmB Nc were irregular in shape with rough surface whereas, grafted AmB Nc were found to be rod-shaped with smooth surface. In vitro drug release of AmB Nc was found to be 86% at the end of one hour. Cellular studies revealed higher invasion and uptake of AmB Nc towards caco-2 cell membrane when compared to ungrafted AmB Nc. Our findings emphasize scope on developing oral delivery system for passively targeting M cells in Peyer’s patches.

Keywords: leishmaniasis, amphotericin b nanocrystals, macrophage targeting, LAS technique

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Authors: M. S. E. Hamroun, K. Bachari, A. Berrayah, L. Mechernene, L. Guerbous

Abstract:

Composite films containing homogeneously dispersed scintillation nano-particles of Lu₂SiO₅:Ce³⁺, in optically transparent polymer matrix, have been prepared and characterized through X-ray diffraction, differential scanning calorimetric (DSC), thermogravimetric analysis (ATG), dynamic mechanical analysis (DMA), electron scanning microscopy morphology (SEM) and photoluminescence (PL). Lu₂SiO₅:Ce³⁺ scintillator powder was successfully synthesized via Sol-Gel method. This study is realized with different mass ratios of nano-particles embedded in polystyrene and polylactic acid polymer matrix (5, 10, 15, 20%) to see the influence of nano-particles on the mechanical, structural and optical properties of films. The composites have been prepared with 400 µm thickness. It has found that the structural proprieties change with mass ratio on each sample. PL photoluminescence shows the characteristic Lu₂SiO₅:Ce³⁺ emission in the blue region and intensity varied for each film.

Keywords: nano-particles, sol gel, photoluminescence, Ce³⁺, scintillator, polystyrene

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Authors: Sijie Chen, Xiaofang Chen, Juan Wang, Yingying Zhang, Yu Hong, Wanyu Zhuang, Xinxin Huang, Ping Ou, Longsheng Huang

Abstract:

Purpose: Autistic symptom improvement can be observed in children treated with acupuncture, but the mechanism is still being explored. In the present study, we used scalp acupuncture to treat autism rat model, and then their improvement in the abnormal behaviors and specific mechanisms behind were revealed by detecting animal behaviors, analyzing the RNA sequencing of the prefrontal cortex(PFC), and observing the ultrastructure of PFC neurons under the transmission electron microscope. Methods: On gestational day 12.5, Wistar rats were given valproic acid (VPA) by intraperitoneal injection, and their offspring were considered to be reliable rat models of autism. They were randomized to VPA or VPA-acupuncture group (n=8). Offspring of Wistar pregnant rats that were simultaneously injected with saline were randomly selected as the wild-type group (WT). VPA_acupuncture group rats received acupuncture intervention at 23 days of age for 4 weeks, and the other two groups followed without intervention. After the intervention, all experimental rats underwent behavioral tests. Immediately afterward, they were euthanized by cervical dislocation, and their prefrontal cortex was isolated for RNA sequencing and transmission electron microscopy. Results: The main results are as follows: 1. Animal behavioural tests: VPA group rats showed more anxiety-like behaviour and repetitive, stereotyped behaviour than WT group rats. While VPA group rats showed less spatial exploration ability, activity level, social interaction, and social novelty preference than WT group rats. It was gratifying to observe that acupuncture indeed improved these abnormal behaviors of autism rat model. 2. RNA-sequencing: The three groups of rats differed in the expression and enrichment pathways of multiple genes related to synaptic function, neural signal transduction, and circadian rhythm regulation. Our experiments indicated that acupuncture can alleviate the major symptoms of ASD by improving these neurological abnormalities. 3. Under the transmission electron microscopy, several lysosomes and mitochondrial structural abnormalities were observed in the prefrontal neurons of VPA group rats, which were manifested as atrophy of the mitochondrial membran, blurring or disappearance of the mitochondrial cristae, and even vacuolization. Moreover, the number of synapses and synaptic vesicles was relatively small. Conversely, the mitochondrial structure of rats in the WT group and VPA_acupuncture was normal, and the number of synapses and synaptic vesicles was relatively large. Conclusion: Acupuncture effectively improved the abnormal behaviors of autism rat model and the ultrastructure of the PFC neurons, which might worked by improving their abnormal synaptic function, synaptic plasticity and promoting neuronal signal transduction.

Keywords: autism spectrum disorder, acupuncture, animal behavior, RNA sequencing, transmission electron microscope

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Authors: Olushola Ayanda, Simphiwe Nelana, Eliazer Naidoo

Abstract:

In the present study, the kinetics, equilibrium and thermodynamics of the adsorption of As(III) ions from aqueous solution onto fly ash (FA) was investigated in batch adsorption system. Prior to the adsorption studies, the FA was characterized by means of x-ray fluorescence (XRF), x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area determination. The effect of contact time, initial As(III) concentration, FA dosage, stirring speed, solution pH and temperature was examined on the adsorption rate. Experimental results showed a very good compliance with the pseudo-second-order equation, while the equilibrium study showed that the sorption of As(III) ions onto FA fitted the Langmuir and Freundlich isotherms. The adsorption process is endothermic and spontaneous, moreover, the maximum percentage removal of As(III) achieved with approx. 2.5 g FA mixed with 25 mL of 100 mg/L As(III) solution was 65.4 % at pH 10, 60 min contact time, temperature of 353 K and a stirring speed of 120 rpm.

Keywords: arsenic, fly ash, kinetics, isotherm, thermodynamics

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Authors: Lise P. Labéjof, Ivna Mororó, Raquel G. Bastos, Maria Isabel G. Severo, Arno H. de Oliveira

Abstract:

This work presents an alternative mode of intestine mucosa renewal that may allow to better understand the total loss of villi after irradiation. It was tested a morphological method of 3d reconstruction using micrographs of serial sections of rat duodenum. We used hundreds of sections of each specimen of duodenum placed on glass slides and examined under a light microscope. Those containing the detachment, approximately a dozen, were chosen for observation under a transmission electron microscope (TEM). Each of these sections was glued on a block of epon resin and recut into a hundred of 60 nm-thick sections. Ribbons of these ultrathin sections were distributed on a series of copper grids in the same order of appearance than during the process of microstomia. They were then stained by solutions of uranyl and lead salts and observed under a TEM. The sections were pictured and the electron micrographs showing signs of cells detachment were transferred into two softwares, ImageJ to align the cellular structures and Reconstruct to realize the 3d reconstruction. It has been detected epithelial cells that exhibited all signs of programmed cell death and localized at the villus-crypt junction. Their nucleus was irregular in shape with a condensed chromatin in clumps. Their cytoplasm was darker than that of neighboring cells, containing many swollen mitochondria. In some places of the sections, we could see intercellular spaces enlarged by the presence of shrunk cells which displayed a plasma membrane with an irregular shape in thermowell as if the cell interdigitations would distant from each other. The three-dimensional reconstruction of the crypts has allowed observe gradual loss of intercellular contacts of crypt cells in the longitudinal plan of the duodenal mucosa. In the transverse direction, there was a gradual increase of the intercellular space as if these cells moved away from one another. This observation allows assume that the gradual remoteness of the cells at the villus-crypt junction is the beginning of the mucosa detachment. Thus, the shrinking of cells due to apoptosis is the way that they detach from the mucosa and progressively the villi also. These results are in agreement with our initial hypothesis and thus have demonstrated that the villi become detached from the mucosa at the villus-crypt junction by the programmed cell death process. This type of loss of entire villus helps explain the rapid denudation of the intestinal mucosa in case of irradiation.

Keywords: 3dr, transmission electron microscopy, ionizing radiations, rat small intestine, apoptosis

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Authors: M. Murmu, Govardhan, J. Satya Eswari

Abstract:

Concrete is the most common and widely used building material. Concrete is basically made of aggregates, both fine and coarse, glued by a cement paste which is made of cement and water. Each one of these constituents of concrete has a negative environmental impact and gives rise to different sustainability issues. The current concrete construction practice is unsustainable because, not only it consumes enormous quantities of stones, sand, and drinking water, but also one billion tons a year of cement, which is not an environment friendly material. Preventing the reduction of natural resources and enhancing the usage of waste materials has become a challenge to the scientist and engineers. A number of studies have been conducted concerning the protection of natural resources, prevention of environmental pollution and contribution to the economy by using this waste material. This paper outlines the influence of Ground Granulated Blast furnace Slag (GGBS) as partial replacement of fine aggregate on mechanical properties of concrete. The strength of concrete is determined having OPC binder, replaced the fine aggregate with15%, 30%, 45% respectively. For this purpose, characteristics concrete mix of M25 with partial replacement of cement with GGBS is used and the strength of concrete cubes and cylinder have determined. The strength of concrete specimens has been compared with the reference specimen. Also X-ray diffraction (XRD) and scanning electron microscope (SEM) tests have been performed to examine the hydration products and the microstructure of the tested specimens. A correlation has been established between the developmental strength concrete with and without GGBS through analysis of hydration products and the microstructure.

Keywords: GGBS, sand, concrete, workability

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Authors: Mahdieh Farzin Asanjan, Erkan Unal Mumcuoglu

Abstract:

Mitochondria are cytoplasmic organelles of the cell, which have a significant role in the variety of cellular metabolic functions. Mitochondria act as the power plants of the cell and are surrounded by two membranes. Significant morphological alterations are often due to changes in mitochondrial functions. A powerful technique in order to study the three-dimensional (3D) structure of mitochondria and its alterations in disease states is Electron microscope tomography. Detection of mitochondria in electron microscopy images due to the presence of various subcellular structures and imaging artifacts is a challenging problem. Another challenge is that each image typically contains more than one mitochondrion. Hand segmentation of mitochondria is tedious and time-consuming and also special knowledge about the mitochondria is needed. Fully automatic segmentation methods lead to over-segmentation and mitochondria are not segmented properly. Therefore, semi-automatic segmentation methods with minimum manual effort are required to edit the results of fully automatic segmentation methods. Here two editing tools were implemented by applying spline surface dragging and interactive live-wire segmentation tools. These editing tools were applied separately to the results of fully automatic segmentation. 3D extension of these tools was also studied and tested. Dice coefficients of 2D and 3D for surface dragging using splines were 0.93 and 0.92. This metric for 2D and 3D for live-wire method were 0.94 and 0.91 respectively. The root mean square symmetric surface distance values of 2D and 3D for surface dragging was measured as 0.69, 0.93. The same metrics for live-wire tool were 0.60 and 2.11. Comparing the results of these editing tools with the results of automatic segmentation method, it shows that these editing tools, led to better results and these results were more similar to ground truth image but the required time was higher than hand-segmentation time

Keywords: medical image segmentation, semi-automatic methods, transmission electron microscopy, surface dragging using splines, live-wire

Procedia PDF Downloads 169