Search results for: scanning electrical microscopy

Authors: Agarana Michael C., Akinlabi Esther T., Pule Kholopane

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In order to sustain the advantages of an advanced manufacturing technique, such as laser sintering, minimization of total processing cost of the parts being produced is very important. An efficient time management would usually very important in optimal cost attainment which would ultimately result in an efficient advanced manufacturing process planning and control. During Laser Scanning Process Scanning (SLS) procedures it is possible to adjust various manufacturing parameters which are used to influence the improvement of various mechanical and other properties of the products. In this study, Modelling and mathematical analysis, including sensitivity analysis, of the laser sintering process time were carried out. The results of the analyses were represented with graphs, from where conclusions were drawn. It was specifically observed that achievement of optimal total scanning time is key for economic efficiency which is required for sustainability of the process.

Keywords: modeling and analysis, optimal planning and control, laser sintering process, scanning time

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Authors: Bing–Jing Zhao, Chang-Kui Liu, Hong Wang, Min Hu

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Electron beam rapid manufacturing (EBRM) or Selective laser melting is an additive manufacturing process that uses 3D CAD data as a digital information source and energy in the form of a high-power laser beam or electron beam to create three-dimensional metal parts by fusing fine metallic powders together.Object:The present study was conducted to evaluate the mechanical properties ,the phase transformation,the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM,SLM and forging technique.Method: Ti-6Al-4V alloy standard test pieces were manufactured by EBRM, SLM and forging technique according to AMS4999,GB/T228 and ISO 10993.The mechanical properties were analyzed by universal test machine. The phase transformation was analyzed by X-ray diffraction and scanning electron microscopy. The corrosivity was analyzed by electrochemical method. The biocompatibility was analyzed by co-culturing with mesenchymal stem cell and analyzed by scanning electron microscopy (SEM) and alkaline phosphatase assay (ALP) to evaluate cell adhesion and differentiation, respectively. Results: The mechanical properties, the phase transformation, the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM、SLM were similar to forging and meet the mechanical property requirements of AMS4999 standard. a­phase microstructure for the EBM production contrast to the a’­phase microstructure of the SLM product. Mesenchymal stem cell adhesion and differentiation were well. Conclusion: The property of the Ti-6Al-4V alloy manufactured by EBRM and SLM technique can meet the medical standard from this study. But some further study should be proceeded in order to applying well in clinical practice.

Keywords: 3D printing, Electron Beam Rapid Manufacturing (EBRM), Selective Laser Melting (SLM), Computer Aided Design (CAD)

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Authors: Ngwenya M., Gumede T. P., Perez Camargo R. A., Motloung B.

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This study presents the development of eco-friendly bio-nanocomposites using poly(lactic acid) (PLA), poly(caprolactone) (PCL), and their blends with nanocellulose extracted from Saccharum Officinarum. The extracted nanocellulose was optimized through chemical treatment and hydrolysis processes, yielding a sustainable and renewable resource for enhancing polymer properties. Bio-nanocomposites of PLA/nanocellulose, PCL/nanocellulose, and PLA/PCL/nanocellulose with varying nanocellulose contents (1, 3, and 5 wt%) were prepared via melt-blending and characterized using Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), dynamic mechanical analysis (DMA) and tensile testing. The results show significant improvements in the thermal and mechanical properties of the polymeric matrices upon the addition of nanocellulose, demonstrating the potential of these bio-nanocomposites for advanced applications. These developments are promising for obtaining bio-nanocomposites from local bio-sources, leading to more sustainable and eco-friendly alternatives to traditional materials.

Keywords: bionanocomposites, polycaprolactone, poly(lactic acid), nanocellulose, saccharum officinarum

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Authors: Azyuni Aziz, Syed A. Malik, Shahrul Kadri Ayop, Fatin Hana Naning

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Currently, organic-inorganic hybrid thin films have attracted researchers to explore them, where these thin films can give a lot of benefits. Hybrid thin films are thin films that consist of inorganic and organic materials. Inorganic and organic materials give high efficiency and low manufacturing cost in some applications such as solar cells application, furthermore, organic materials are environment-friendly. In this study, poly (3-hexylthiophene) was choosing as organic material which combined with inorganic nanoparticles, Cadmium Sulfide (CdS) quantum dots. Samples were prepared using new technique, Angle Lifting Deposition (ALD) at different weight percentage. All prepared samples were then characterized by Field Emission Scanning Electron Microscopy (FESEM) with Energy-dispersive X-ray spectroscopy (EDX) and Atomic Force Microscopy (AFM) to study surface of samples and determine their surface roughness. Results show that these inorganic nanoparticles have affected the surface of samples and surface roughness of samples increased due to increasing of weight percentage of CdS in the thin films samples.

Keywords: AFM, CdS, FESEM-EDX, hybrid thin films, P3HT

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Authors: Picha Sriprachan

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The increase in electricity prices affects the cost of high-rise building construction. The objectives of this research are to study the electrical cost, trend of electrical cost and to forecast electrical cost of high-rise building construction. The methods of this research are: 1) to study electrical payment formats, cost data collection methods, and the factors affecting electrical cost of high-rise building construction, 2) to study the quantity and trend of cumulative percentage of the electrical cost, and 3) to forecast the electrical cost for different types of high-rise buildings. The results of this research show that the average proportion between electrical cost and the value of the construction project is 0.87 percent. The proportion of electrical cost for residential, office and commercial, and hotel buildings are closely proportional. If construction project value increases, the proportion of electrical cost and the value of the construction project will decrease. However, there is a relationship between the amount of electrical cost and the value of the construction project. During the structural construction phase, the amount of electrical cost will increase and during structural and architectural construction phase, electrical cost will be maximum. The cumulative percentage of the electrical cost is related to the cumulative percentage of the high-rise building construction cost in the same direction. The amount of service space of the building, number of floors and the duration of the construction affect the electrical cost of construction. The electrical cost of construction forecasted by using linear regression equation is close to the electrical cost forecasted by using the proportion of electrical cost and value of the project.

Keywords: high-rise building construction, electrical cost, construction phase, architectural phase

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Authors: Ezgi Yurdakul, Klaus-Alexander Rieder, Richard Sibbick

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Most of the shotcrete projects require compliance with meeting a specified early-age strength target (e.g., reaching 1 MPa in 1 hour) that is selected based on the underground conditions. To meet the desired early-age performance characteristics, accelerators are commonly used as they increase early-age strength development rate and accelerate the setting thereby reducing sagging and rebound. The selection of accelerator type and its dosage is made by the setting time and strength required for the shotcrete application. While alkaline and alkali-free accelerators are the two main types used in wet-mix shotcrete; alkali-free admixtures increasingly substitute the alkaline accelerators to improve the performance and working safety. This paper aims to evaluate the impact of alkali-free accelerators in wet-mix on various tests including set time, early and later-age compressive strength, boiled absorption, and electrical resistivity. Furthermore, the comparison between accelerated and non-accelerated samples will be made to demonstrate the interaction between cement and accelerators. Scanning electron microscopy (SEM), fluorescent resin impregnated thin section and cut and polished surface images will be used to understand the microstructure characterization of mixes in the presence of accelerators.

Keywords: accelerators, chemical admixtures, shotcrete, sprayed concrete

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Authors: D. Benmoussa, H. Hannache, O. Cherkaoui

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In textiles, the major interest in microencapsulation is currently in the application of durable fragrances, skin softeners, phase-change materials, antimicrobial agents and drug delivery systems onto textile materials. In our research “Polyethylene Glycol” was applied as phase change material and it was encapsulated in polymethacrylic acid (PMA) by radical polymerization in suspension of methacrylic acid in presence of N,N'-methylenebisacrylamide (MBAM) as crosslinking agent. Thereafter the obtained microcapsule was modified by amidation with ethylenediamine as a spacer molecule. At the end of this spacer trichlorotriazine reactive group was fixed. Microcapsules were grafted onto cotton textile substrate. The surface morphologies of the microencapsulated phase change materials (micro PCMs) were studied by scanning electron microscopy (SEM). Thermal properties, thermal reliabilities and thermal stabilities of the as-prepared micro PCMs were investigated by differential scanning calorimetry (DSC) and thermogravmetric analysis (TGA). The results obtained show the obtaining microcapsules with a mean diameter of 10 µm and the resistance of the microcapsules is demonstrated by thermal analysis.

Keywords: energy storage, microencapsulation, phase-change materials, thermogravmetric analysis (TGA)

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Authors: Kenny Onayemi

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In an era where academic institutions increasingly rely on information technology, the security of academic networks has emerged as a paramount concern. This comprehensive study delves into the effectiveness of security practices, including network mapping, vulnerability scanning, and penetration testing, within academic networks. Leveraging data from surveys administered to faculty, staff, IT professionals and IT students in the university, the study assesses their familiarity with these practices, perceived effectiveness, and frequency of implementation. The findings reveal that a significant portion of respondents exhibit a strong understanding of network mapping, vulnerability scanning, and penetration testing, highlighting the presence of knowledgeable professionals within academic institutions. Additionally, active scanning using network scanning tools and automated vulnerability scanning tools emerge as highly effective methods. However, concerns arise as the respondents show that the academic institutions conduct these practices rarely or never. Notably, many respondents have reported significant vulnerabilities or security incidents through these security measures within their institution. This study concludes with recommendations to enhance network security awareness and practices among faculty, staff, IT personnel, and students, ultimately fortifying the security posture of academic networks in the digital age.

Keywords: network security, academic networks, vulnerability scanning, penetration testing, information security

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Authors: Babak Eslami

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Bimodal and trimodal AFM have provided additional capabilities to scanning probe microscopy characterization techniques. These capabilities have specifically enhanced material characterization of surfaces and provided subsurface imaging in addition to conventional topography images. Bimodal and trimodal AFM, being different techniques of multifrequency AFM, are based on exciting the cantilever’s fundamental eigenmode with second and third eigenmodes simultaneously. Although higher eigenmodes provide a higher number of observables that can provide additional information about the sample, they cause experimental challenges. In this work, different experimental approaches for enhancing AFM images in multifrequency for different characterization goals are provided. The trade-offs between eigenmodes including the advantages and disadvantages of using each mode for different samples (ranging from stiff to soft matter) in both air and liquid environments are provided. Additionally, the advantage of performing conventional single tapping mode AFM with higher eigenmodes of the cantilever in order to reduce sample indentation is discussed. These analyses are performed on widely used polymers such as polystyrene, polymethyl methacrylate and air nanobubbles on different surfaces in both air and liquid.

Keywords: multifrequency, sensitivity, soft matter, polymer

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Authors: O. I. H. Dimitry, N. A. Mansour, A. L. G. Saad

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Natural sodium montmorillonite (NaMMT), Cloisite Na⁺ and two organophilic montmorillonites (OMMTs), Cloisites 20A and 15A were used. Polycaprolactone (PCL)/MMT composites containing 1, 3, 5, and 10 wt% of Cloisite Na⁺ and PCL/OMMT nanocomposites containing 5 and 10 wt% of Cloisites 20A and 15A were prepared via solution intercalation technique to study the influence of organic modifier loading on particle dispersion of PCL/ NaMMT composites. Thermal stabilities of the obtained composites were characterized by thermal analysis using the thermogravimetric analyzer (TGA) which showed that in the presence of nitrogen flow the incorporation of 5 and 10 wt% of filler brings some decrease in PCL thermal stability in the sequence: Cloisite Na+>Cloisite 15A > Cloisite 20A, while in the presence of air flow these fillers scarcely influenced the thermoxidative stability of PCL by slightly accelerating the process. The interaction between PCL and silicate layers was studied by Fourier transform infrared (FTIR) spectroscopy which confirmed moderate interactions between nanometric silicate layers and PCL segments. The electrical conductivity (σ) which describes the ionic mobility of the systems was studied as a function of temperature and showed that σ of PCL was enhanced on increasing the modifier loading at filler content of 5 wt%, especially at higher temperatures in the sequence: Cloisite Na⁺<Cloisite 20A<Cloisite 15A, and was then decreased to some extent with a further increase to 10 wt%. The activation energy E_σ obtained from the dependency of σ on temperature using Arrhenius equation was found to be lowest for the nanocomposite containing 5 wt% of Cloisite 15A. The dispersed behavior of clay in PCL matrix was evaluated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses which revealed partial intercalated structures in PCL/NaMMT composites and semi-intercalated/semi-exfoliated structures in PCL/OMMT nanocomposites containing 5 wt% of Cloisite 20A or Cloisite 15A.

Keywords: electrical conductivity, montmorillonite, nanocomposite, organoclay, polycaprolactone

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Authors: Raana Babadi Fathipour

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Hydrogels are three-dimensional structures formed by the interweaving of polymeric materials, possessing the remarkable ability to imbibe copious amounts of water. Numerous methodologies have been devised for examining and understanding the properties of these synthesized gels. Amongst them, spectroscopic techniques such as ultraviolet/visible (UV/Vis) and Fourier-transform infrared (FTIR) spectroscopy offer a glimpse into molecular and atomic aspects. Additionally, diffraction methods like X-ray diffraction (XRD) enable one to measure crystallinity within the gel's structure, while microscopy tools encompassing scanning electron microscopy (SEM) and transmission electron microscopy (TEM) provide insights into surface texture and morphology. Furthermore, rheology serves as an invaluable tool for unraveling the viscoelastic behavior inherent in hydrogels—a parameter crucial not only to numerous industries, including pharmaceuticals, cosmetics, food processing, agriculture and water treatment, but also pivotal to related fields of research. Likewise, the ultimate configuration of the product is contingent upon its characterization at a microscopic scale in order to comprehend the intricacies of the hydrogel network's structure and interaction dynamics in response to external forces. Within this present scrutiny, our attention has been devoted to unraveling the intricate rheological tendencies exhibited by materials founded on synthetic, natural, and semi-synthetic hydrogels. We also explore their practical utilization within various facets of everyday life from an industrial perspective.

Keywords: rheology, hydrogels characterization, viscoelastic behavior, application

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

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Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: ceramics, energy storage, electrochemical measurements, transmission electron microscope

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Authors: Aynur Aker, Hasan Kaya

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In recent years, the use of the aluminum based alloys in the industry and technology are increasing. Alloying elements in aluminum have further been improving the strength and stiffness properties that provide superior compared to other metals. In this study, investigation of physical properties (microstructure, microhardness, tensile strength, electrical conductivity and thermal properties) in the Al-12.6wt.%Si-%2wt.Ni ternary alloy were investigated. Al-Si-Ni alloy was prepared in a graphite crucible under vacuum atmosphere. The samples were directionally solidified upwards with different growth rate (V) at constant temperature gradient G (7.73 K/mm). The microstructures (flake spacings, λ), microhardness (HV), ultimate tensile strength, electrical resistivity and thermal properties enthalpy of fusion and specific heat and melting temperature) of the samples were measured. Influence of the growth rate and flake spacings on microhardness, ultimate tensile strength and electrical resistivity were investigated and relationships between them were experimentally obtained by using regression analysis. According to results, λ values decrease with increasing V, but microhardness, ultimate tensile strength, electrical resistivity values increase with increasing V. Variations of electrical resistivity for cast samples with the temperature in the range of 300-1200 K were also measured by using a standard dc four-point probe technique. The enthalpy of fusion and specific heat for the same alloy was also determined by means of differential scanning calorimeter (DSC) from heating trace during the transformation from liquid to solid. The results obtained in this work were compared with the previous similar experimental results obtained for binary and ternary alloys.

Keywords: electrical resistivity, enthalpy, microhardness, solidification, tensile stress

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Authors: Yasser A. Ahmed, Juleen M Dickson, Evan S. Krystofiak, Julie A. Oliver

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Cancer cells urgently need folate to support their rapid division. Folate receptors (FR) are over-expressed on a wide range of tumor cells, including breast cancer cells. FR are distributed over the entire surface of cancer cells, but are polarized to the apical surface of normal cells. Targeting of cancer cells using specific surface molecules such as folate receptors may be one of the strategies used to kill cancer cells without hurting the neighing normal cells. The aim of the current study was to try a method of SEM detecting FR in a murine breast cancer cell model (4T1 cells) using secondary antibody conjugated to gold or gold-coated magnetite nanoparticles. 4T1 cells were suspended in RPMI medium witth FR antibody and incubated with secondary antibody for fluorescence microscopy. The cells were cultured on 30mm Thermanox coverslips for 18 hours, labeled with FR antibody then incubated with secondary antibody conjugated to gold or gold-coated magnetite nanoparticles and processed to scanning electron microscopy (SEM) analysis. The fluorescence microscopy study showed strong punctate FR expression on 4T1 cell membrane. With SEM, the labeling with gold or gold-coated magnetite conjugates showed a similar pattern. Specific labeling occurred in nanoparticle clusters, which are clearly visualized in backscattered electron images. The 4T1 tumor cell model may be useful for the development of FR-targeted tumor therapy using gold-coated magnetite nano-particles.

Keywords: cancer cell, nanoparticles, cell culture, SEM

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Authors: Rashad Al-Gaashani, Muataz A. Atieh

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In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

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Authors: Gopal Ji, Priyanka Dwivedi, Shanthi Sundaram, Rajiv Prakash

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Inhibition effect of aqueous Argemone Mexicana root extract (AMRE) on mild steel corrosion in 1 M HCl has been studied by weight loss, Tafel polarization curves, electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. Results indicate that inhibition ability of AMRE increases with the increasing amount of the extract. A maximum corrosion inhibition of 94% is acknowledged at the extract concentration of 400 mg L-1. Polarization curves and impedance spectra reveal that both cathodic and anodic reactions are suppressed due to passive layer formation at metal-acid interface. It is also confirmed by SEM micro graphs and FTIR studies. Furthermore, the effects of acid concentration (1-5 M), immersion time (120 hours) and temperature (30-60˚C) on inhibition potential of AMRE have been investigated by weight loss method and electrochemical techniques. Adsorption mechanism is also proposed on the basis of weight loss results, which shows good agreement with Langmuir isotherm.

Keywords: mild steel, polarization, SEM, acid corrosion, EIS, green inhibition

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Authors: Sharan K. Indrakar, Aakash B. Prasad, Arash Takshi, Sesha Srinivasan, Elias K. Stefanakos

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In this work, we present an exclusive study on the effect of the feeding ratio of polyaniline-based redox-active gel layer on electrical and optical properties of innovative electrochromic devices (ECs). An electrochromic device consisting of polyaniline (PANI) has a redox-active gel electrolyte placed between two conducting transparent fluorine-doped tin oxide glass substrates. The redox-active composite gel is a mixture of different concentrations of aniline (monomer), a water-soluble polymer poly (vinyl alcohol), hydrochloric acid, and an oxidant. The EC device shows the color change from dark green to transparent for the applied potential between -0.5 V to +2.0 V. The coloration and decoloration of the ECs were tested for electrochemical behavior using techniques such as cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS). The optical transparency of the EC devices was examined at two different biasing voltage conditions under UV-visible spectroscopic technique; the result showed 65% transmittance at 564 nm and zero transmittance when the cell was biased at 0.0 V and 2.0 V, the synthesized mol fraction gel was analyzed for surface morphology and structural properties by scanning electron microscopy and Fourier transformer spectroscopy.

Keywords: electrochromic, gel electrolyte, polyaniline, conducting polymer

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Authors: A. E. Delgado, W. Aperador

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This study evaluated the incidence of concentrated natural fibre, as well as the effects of adding a crosslinking agent on the torque when those components are mixed with low density polyethylene (LDPE). The natural fibre has a particle size of between 0.8-1.2mm and a moisture content of 0.17%. An internal mixer was used to measure the torque required to mix the polymer with the fibre. The effect of the fibre content and crosslinking agent on the torque was also determined. A change was observed in the morphology of the mixes using SEM differential scanning microscopy.

Keywords: WPC, DCP, LDPE, natural fibre, torque

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Authors: Shalini Rajput, Dinesh Mohan

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Water is the most important and essential resources for existing of life on the earth. Water quality is gradually decreasing due to increasing urbanization and industrialization and various other developmental activities. It can pose a threat to the environment and public health therefore it is necessary to remove hazardous contaminants from wastewater prior to its discharge to the environment. Recently, magnetic iron oxide nanoparticles have been arise as significant materials due to its distinct properties. This article focuses on the synthesis method with a possible mechanism, structure and application of magnetic iron oxide nanoparticles. The various characterization techniques including X-ray diffraction, transmission electron microscopy, scanning electron microscopy with energy dispersive X-ray, Fourier transform infrared spectroscopy and vibrating sample magnetometer are useful to describe the physico-chemical properties of nanoparticles. Nanosized iron oxide particles utilized for remediation of contaminants from aqueous medium through adsorption process. Due to magnetic properties, nanoparticles can be easily separate from aqueous media. Considering the importance and emerging trend of nanotechnology, iron oxide nanoparticles as nano-adsorbent can be of great importance in the field of wastewater treatment.

Keywords: nanoparticles, adsorption, iron oxide, nanotechnology

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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: Ana Carolina Kogawa, Selma Gutierrez Antonio, Hérida Regina Nunes Salgado

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Rifaximin is an oral antimicrobial, gut - selective and not systemic with adverse effects compared to placebo. It is used for the treatment of hepatic encephalopathy, travelers diarrhea, irritable bowel syndrome, Clostridium difficile, ulcerative colitis and acute diarrhea. The crystalline form present in the rifaximin with minimal systemic absorption is α, being the amorphous form significantly different. Regulators are increasingly attention to polymorphisms. Polymorphs can change the form by altering the drug characteristics compromising the effectiveness and safety of the finished product. International Conference on Harmonization issued the ICH Guidance Q6A, which aim to improve the control of polymorphism in new and existing pharmaceuticals. The objective of this study was to obtain polymorphic forms of rifaximin employing recrystallization processes and characterize them by thermal analysis (thermogravimetry - TG and differential scanning calorimetry - DSC), X-ray diffraction, scanning electron microscopy and solubility test. Six polymorphic forms of rifaximin, designated I to VI were obtained by the crystallization process by evaporation of the solvent. The profiles of the TG curves obtained from polymorphic forms of rifaximin are similar to rifaximin and each other, however, the DTG are different, indicating different thermal behaviors. Melting temperature values of all the polymorphic forms were greater to that shown by the rifaximin, indicating the higher thermal stability of the obtained forms. The comparison of the diffractograms of the polymorphic forms of rifaximin with rifaximin α, β and γ constant in patent indicate that forms III, V and VI are formed by mixing polymorph β and α and form III is formed by polymorph β. The polymorphic form I is formed by polymorph β, but with a significant amount of amorphous material. Already, the polymorphic form II consists of polymorph γ, amorphous. In scanning electron microscope is possible to observe the heterogeneity of morphological characteristics of crystals of polymorphic forms among themselves and with rifaximin. The solubility of forms I and II was greater than the solubility of rifaximin, already, forms III, IV and V presented lower solubility than of rifaximin. Similarly, the bioavailability of the amorphous form of rifaximin is considered significantly higher than the form α, the polymorphic forms obtained in this work can not guarantee the excellent tolerability of the reference medicine. Therefore, studies like these are extremely important and they point to the need for greater requirements by the regulatory agencies competent about polymorphs analysis of the raw materials used in the manufacture of medicines marketed globally. These analyzes are not required in the majority of official compendia. Partnerships between industries, research centers and universities would be a viable way to consolidate researches in this area and contribute to improving the quality of solid drugs.

Keywords: electronic microscopy, polymorphism, rifaximin, solubility, X-ray diffraction

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Authors: Somayeh Azizi, Mohammad Hossein Ehsani, Amir Zareidoost

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In this research, a technique has been developed to reduce the corrosion rate of magnesium (Mg) metal by creating Zr-Nb thin film coatings. In this regard, thin-film coatings of niobium (Nb) zirconium (Zr) double alloy are applied on pure Mg specimens under different processes conditions, such as the change of the substrate temperature, substrate bias, and coating thickness using the magnetron sputtering method. Then, deposited coatings are analyzed in terms of surface features via field-emission scanning electron microscopy (FE-SEM), thin-layer X-ray diffraction (GI-XRD), energy-dispersive X-ray spectroscopy (EDS), atomic force microscopy (AFM), and corrosion tests. Also, nano-scratch tests were carried out to investigate the adhesion of the thin film. The results showed that the (Zr-Nb) thin films could control the degradation rate of Mg in the simulated body fluid (SBF). The nano-scratch studies depicted that the (Zr-Nb) thin films have a proper adhesion with the Mg substrate. Therefore, this technique could be used to enhance the corrosion resistance of bare Mg and could result in improving the performance of the biodegradable Mg implant for orthopedic applications.

Keywords: (Zr-Nb) thin film, magnetron sputtering, biodegradable Mg, degradation rate

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Authors: Tatiana Franco, Hugo A. Estupinan

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Banana pseudostem fiber (BPF) and pineapple leaf fiber (PLF) for their excellent mechanical properties and biodegradability characteristics arouse interest in different areas of research. F In tropical regions, where the banana pseudostem and the pineapple leaf are transformed into hard-to-handle solid waste, they can be low-cost raw material and environmentally sustainable in research for composite materials. In terms of functionality of this type of fiber, an open structure would allow the adsorption and retention of organic, inorganic and metallic species. In general, natural fibers have closed structures on their surface with intricate internal arrangements that can be used for the solution of environmental problems and other technological uses, however it is not possible to access their internal structure and sublayers, exposing the fibers in the natural state. An alternative method to chemical and enzymatic treatment are the processes with the plasma treatments, which are known to be clean, economical and controlled. In this type of treatment, a gas contained in a reactor in the form of plasma acts on the fiber generating changes in its structure, morphology and topography. This work compares the effects on fibers of PLF and BPF treated with cold argon plasma, alternating time and current. These fibers are grown in the regions of Antioquia-Colombia. The morphological, compositional and wettability properties of the fibers were analyzed by Raman microscopy, contact angle measurements, scanning electron microscopy (SEM) and atomic force microscopy analysis (AFM). The treatment with cold plasma on PLF and BPF allowed increasing its wettability, the topography and the microstructural relationship between lignin and cellulose.

Keywords: cold plasma, contact angle, natural fibers, Raman, SEM, wettability

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

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

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

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: electron diffraction spectroscopy, high strength concrete, interfacial transition zone, normal strength concrete, scanning electron microscopy

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Authors: H. M. Fayzan Shakir, Khadija Zubair, Tingkai Zhao

Abstract:

Electromagnetic (EM) waves are being used widely now a days. Cell phone signals, WIFI signals, wireless telecommunications etc everything uses EM waves which then create EM pollution. EM pollution can cause serious effects on both human health and nearby electronic devices. EM waves have electric and magnetic components that disturb the flow of charged particles in both human nervous system and electronic devices. The shielding of both humans and electronic devices are a prime concern today. EM waves can cause headaches, anxiety, suicide and depression, nausea, fatigue and loss of libido in humans and malfunctioning in electronic devices. Polyaniline (PANI) and polypyrrole (PPY) were successfully synthesized using chemical polymerizing using ammonium persulfate and DBSNa as oxidant respectively. Barium ferrites (BaFe) were also prepared using co-precipitation method and calcinated at 10500C for 8h. Nanocomposite thin films with various combinations and compositions of Polyvinylchloride, PANI, PPY and BaFe were prepared. X-ray diffraction technique was first used to confirm the successful fabrication of all nano fillers and particle size analyzer to measure the exact size and scanning electron microscopy is used for the shape. According to Electromagnetic Interference theory, electrical conductivity is the prime property required for the Electromagnetic Interference shielding. 4-probe technique is then used to evaluate DC conductivity of all samples. Samples with high concentration of PPY and PANI exhibit remarkable increased electrical conductivity due to fabrication of interconnected network structure inside the Polyvinylchloride matrix that is also confirmed by SEM analysis. Less than 1% transmission was observed in whole NIR region (700 nm – 2500 nm). Also, less than -80 dB Electromagnetic Interference shielding effectiveness was observed in microwave region (0.1 GHz to 20 GHz).

Keywords: nanocomposites, polymers, EMI shielding, thermal imaging

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Authors: Eman Alzahrani

Abstract:

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

Keywords: chitosan, magnetic nanoparticles, coprecipitation, adsorption

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Authors: Chao Hu, Xinwen Liao, Qing-Hua Qin, Gang Wang

Abstract:

The hierarchical carbon nanotube (CNT)/carbon fiber (CF)/high density polyethylene (HDPE) was fabricated via compound extrusion and injection molding, in which to author’s best knowledge CNT was employed as a nano-coatings on the surface of CF for the first time by spray coating technique. The CNT coatings relative to CF was set at 1 wt% and the CF content relative to the composites varied from 0 to 25 wt% to study the influence of CNT coatings and CF contents on the mechanical, thermal and morphological performance of this hierarchical composites. The results showed that with the rise of CF contents, the mechanical properties, including the tensile properties, flexural properties, and hardness of CNT/CF/HDPE composites, were effectively improved. Furthermore, the CNT-coated composites showed overall higher mechanical performance than the uncoated counterparts. It can be ascribed to the enhancement of interfacial bonding between the CF and HDPE via the incorporation of CNT, which was demonstrated by the scanning electron microscopy observation. Meanwhile, the differential scanning calorimetry data indicated that by the introduction of CNT and CF, the crystallization temperature and crystallinity of HDPE were affected while the melting temperature did not have an obvious alteration.

Keywords: carbon fibers, carbon nanotubes, extrusion, high density polyethylene

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Authors: Amine Mezni, Merfat Algethami, Ali Aldalbahi, Arwa Alrooqi, Abel Santos, Dusan Losic, Sarah Alharthi, Tariq Altalhi

Abstract:

In situ synthesis of carbon nanotubes featuring different diameters (10-200 nm), lengths (1 to 100 µm) and periodically nanostructured shape was performed in a custom designed chemical vapor deposition (CVD) system using nanoporous anodic alumina (NAA) under different conditions. The morphology of the resulting CNTs/NAA composites and free-standing CNTs were analyzed by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results confirm that highly ordered arrays of CNTs with precise control of nanotube dimensions in the range 20-200 nm with tube length in the range < 1 µm to > 100 μm and with periodically shaped morphology can be fabricated using nanostructured NAA templates prepared by anodization. This technique allows us to obtain tubes open at one / both ends with a uniform diameter along the pore length without using any metal catalyst. Our finding suggests that this fabrication strategy for designing new CNTs membranes and structures can be significant for emerging applications as molecular separation/transport, optical biosensing, and drug delivery.

Keywords: carbon nanotubes, CVD approach, composites membrane, nanoporous anodic alumina

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Authors: Folorunso Omoniyi, Peter Olubambi, Rotimi Sadiku

Abstract:

Thermal barrier coating (TBC) system is used in both aero engines and other gas turbines to offer oxidation protection to superalloy substrate component. In the present work, it shows the ability of a new fabrication technique to develop rapidly new coating composition and microstructure. The compact powders were prepared by Powder Metallurgy method involving powder mixing and the bond coat was synthesized through the application of Spark Plasma Sintering (SPS) at 10500C to produce a fully dense (97%) NiCrAl bulk samples. The influence of sintering temperature on the hardness of NiCrAl, done by Micro Vickers hardness tester, was investigated. And Oxidation test was carried out at 1100oC for 20h, 40h, and 100h. The resulting coat was characterized with optical microscopy, scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDAX) and x-ray diffraction (XRD). Micro XRD analysis after the oxidation test revealed the formation of protective oxides and non-protective oxides.

Keywords: high-temperature oxidation, powder metallurgy, spark plasma sintering, thermal barrier coating

Procedia PDF Downloads 478