Search results for: high resolution transmission electron microscopy

Authors: C. L. Popa, S. L. Iconaru, A. Costescu, C. S. Ciobanu, M. Motelica Heino, R. Guegan, D. Predoi

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Surface functionalization of ceramic composites with a special focus on tetraethyl orthosilicate (TEOS) and hydroxyapatite (HAp) is discoursed. Mesoporous ceramic HAp-TEOS composites were prepared by the incorporation of hydroxyapatite into tetraethyl orthosilicate by sol-gel method. The resulting samples were analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and Raman spectroscopy and nitrogen physisorption. The removal of Pb2+ ions from aqueous solutions was evaluated using Atomic Absorbtion Spectroscopy (AAS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled Pb2+ at pH ~ 3 and pH ~ 5. After removal experiment of Pb2+ at pH 3 and pH 5, porous hydroxyapatite nanoparticles is transformed into PbHAp_3 and PbHAp_5 via the adsorption of Pb2+ ions followed by the cation exchange reaction. The diffraction patterns show that THAp nanoparticles were successfully coated with teos without any structural changes. On the other, the AAS analysis showed that THAp can be useful in the removal Pb2+ from water contaminated.

Keywords: teos, hydroxyapatite, environment applications, biosystems engineering

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Authors: Mechri hanane, Azzaz Mohammed

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Polycrystalline CuFe thin film was prepared by thermal evaporation process (Physical vapor deposition), using the nanocrystalline CuFe powder obtained by mechanical alloying After 24 h of milling elemental powders. The microscopic study of nanocrystalline powder and the thin film of Cu70Fe30 binary alloy were examined using transmission electron microscopy (TEM) and scanning electron microscope (SEM). The cross-sectional TEM images showed that the obtained CuFe layer was polycrystalline film of about 20 nm thick and composed of grains of different size ranging from 4 nm to 18 nm.

Keywords: nanomaterials, thin films, TEM, SEM

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Authors: Stephen Rathinaraj Benjamin, Flavio Colmati Junior, Maria Izabel Florindo Guedes, Rosa Amalia Fireman Dutra

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A new enzymatic electrochemical biosensor based on multiwall carbon nanotubes and cerium oxide nanoparticles for the detection of rutin has been developed. The cerium oxide nanoparticles /HRP/ multiwall carbon nanotubes/ carbon paste electrode (HRP/ CeO2/MWCNTs/CPE) was prepared by ensuing addition of MWCNTs and HRP on the CPE, followed by the mixing with cerium oxide nanoparticles. Surface physical characteristics of the modified electrode and the electrochemical properties of the composite were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), cylic voltammetry (CV), differential pulse voltammetry (DPV) and square wave voltammetry (SWV). The HRP/ CeO2/MWCNTs/CPE showed good selectivity, stability and reproducibility, which was further applied to detect rutin tablet and capsule samples with satisfactory results.

Keywords: cerium dioxide nanoparticles, horseradish peroxidase, multiwall carbon nanotubes, rutin

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Authors: Seyedmahdi Mousavihashemi

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Natural Akermanite (NAM) has been successfully prepared by a modified sol-gel method. Optimization in calcination temperature and mechanical ball milling resulted in a pure and nano-sized powder which characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared Spectroscopy (FT–IR). We hypothesized that nano-sized Akermanite (AM) would mimic more efficiently the nanocrystal structure and function of natural bone apatite, owing to the higher surface area, compare to conventional micron-size Akermanite (AM). Accordingly, we used the unique advantage of nanotechnology to improve novel nano akermanite particles as a potential candidate for bone tissue regeneration whether as a per implant filling powder or in combination with other biomaterials as a composite scaffold. Pure Akermanite (PAM) powders were successfully obtained via a simple sol-gel method followed by calcination at 1250 °C. Mechanical grinding in a ceramic ball mill for 7 hours resulted in akermanite (AM) nanoparticles in the range of about 30- 45 nm.

Keywords: biomedical engineering, nano composite, SEM, TEM

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Authors: M. Haghnegahdar, G. Naderi, M. H. R. Ghoreishy

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Polypropylene(PP)/Ethylene Propylene Diene Monomer (EPDM) samples (80/20) containing 0, 0.5, 1, 1.5, 2, 2.5, and 3 (expressed in mass fraction) graphene were prepared using melt compounding method to investigate microstructure, mechanical properties, and thermal stability as well as electrical resistance of samples. X-Ray diffraction data confirmed that graphene platelets are well dispersed in PP/EPDM. Mechanical properties such as tensile strength, impact strength and hardness demonstrated increasing trend by graphene loading which exemplifies substantial reinforcing nature of this kind of nano filler and it's good interaction with polymer chains. At the same time it is found that thermo-oxidative degradation of PP/EPDM nanocomposites is noticeably retarded with the increasing of graphene content. Electrical surface resistivity of the nanocomposite was dramatically changed by forming electrical percolation threshold and leads to change electrical behavior from insulator to semiconductor. Furthermore, these results were confirmed by scanning electron microscopy(SEM), dynamic mechanical thermal analysis (DMTA), and transmission electron microscopy (TEM).

Keywords: nanocomposite, graphene, microstructure, mechanical properties

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Authors: Przemyslaw J. Jodlowski, Roman J. Jedrzejczyk, Damian K. Chlebda, Anna Dziedzicka, Lukasz Kuterasinski, Anna Gancarczyk, Maciej Sitarz

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The aim of this study was to obtain highly active catalysts based on non-noble metal oxides supported on zirconia prepared via a sonochemical method. In this study, the influence of the stabilizers addition during the preparation step was checked. The final catalysts were characterized by using such characterization methods as X-ray Diffraction (XRD), nitrogen adsorption, X-ray fluorescence (XRF), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and µRaman. The proposed preparation method allowed to obtain uniformly dispersed metal-oxide nanoparticles at the support’s surface. The catalytic activity of prepared catalyst samples was measured in a methane combustion reaction. The activity of the catalysts prepared by the sonochemical method was considerably higher than their counterparts prepared by the incipient wetness method.

Keywords: methane catalytic combustion, nanoparticles, non-noble metals, sonochemistry

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Authors: Songyan Yin, Ravindra Rajarao, Veena Sahajwalla

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Automotive plastics waste (widely known as auto-fluff or ASR) is a complicated mixture of various plastics incorporated with a wide range of additives and fillers like titanium dioxide, magnesium oxide, and silicon dioxide. Automotive plastics waste is difficult to recycle and its landfilling poses the significant threat to the environment. In this study, a sustainable technology to fabricate protective nanoscale TiN thin film on a steel substrate surface by using automotive waste plastics as titanium and carbon resources is suggested. When heated automotive plastics waste with steel at elevated temperature in a nitrogen atmosphere, titanium dioxide contented in ASR undergo carbothermal reduction and nitridation reactions on the surface of the steel substrate forming a nanoscale thin film of titanium nitride on the steel surface. The synthesis of TiN film on steel substrate under this technology was confirmed by X-ray photoelectron spectrometer, high resolution X-ray diffraction, field emission scanning electron microscope, a high resolution transmission electron microscope fitted with energy dispersive X-ray spectroscopy, and inductively coupled plasma mass spectrometry techniques. This sustainably fabricated TiN film was verified of dense, well crystallized and could provide good oxidation resistance to the steel substrate. This sustainable fabrication technology is maneuverable, reproducible and of great economic and environmental benefit. It not only reduces the fabrication cost of TiN coating on steel surface, but also provides a sustainable environmental solution to recycling automotive plastics waste. Moreover, high value copper droplets and char residues were also extracted from this unique fabrication process.

Keywords: automotive plastics waste, carbonthermal reduction and nitirdation, sustainable, TiN film

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Authors: Tlotlollo Sidwell Hlalele, Shengzhi Du

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High voltage transmission is the most pivotal process in the electrical power industry. It requires a robust infrastructure that can last for decades without causing impairment in human life. Due to the so-called global warming, power transmission system has started to experience some challenges which could presumably escalate more in future. These challenges are earthquake resistance, transmission power losses, and high electromagnetic field. In this paper, research efforts aim to address these challenges are discussed. We focus in particular on the research in regenerative electric energy such as: wind, hydropower, biomass and sea-waves based on the energy storage and transmission possibility. We conclude by drawing attention to specific areas that we believe need more research.

Keywords: power transmission, regenerative energy, power quality, energy storage

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Authors: S. Melvin Samuel, Jayanta Bhattacharya

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In the present study, a graphene oxide/chitosan (GO-CS) composite material was prepared and used as an adsorbent for the removal of methylene blue (MB) from aqueous solution. The synthesized GO-CS adsorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopes (SEM), transmission electron microscopy (TEM), Raman spectroscopy and thermogravimetric analysis (TGA). The removal of MB was conducted in batch mode. The effect of parameters influencing the adsorption of MB such as pH of the solution, initial MB concentration, shaking speed, contact time and adsorbent dosage were studied. The results showed that the GO-CS composite material has high adsorption capacity of 196 mg/g of MB solution at pH 9.0. Further, the adsorption of MB on GO-CS followed pseudo second order kinetics and equilibrium adsorption data well fitted by the Langmuir isotherm model. The study suggests that the GO-CS is a favorable adsorbent for the removal of MB from aqueous solution.

Keywords: Methylene blue, Graphene oxide-chitosan, Isotherms, Kinetics.

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Authors: Khurram Munir, Cuie Wen, Yuncang Li

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Magnesium (Mg) metal matrix composites (MMCs) reinforced with graphene nanoplatelets (GNPs) have been developed by powder metallurgy (PM). In this study, GNPs with different concentrations (0.1-0.3 wt.%) were dispersed into Mg powders by high-energy ball-milling processes. The microstructure and resultant mechanical properties of the fabricated nanocomposites were characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy (RS), compression and nano-wear tests. The corrosion resistance of the fabricated composites was evaluated by electrochemical tests and hydrogen evolution measurements. Finally, the biological response of Mg-GNPs composites was assessed using osteoblast-like SaOS2 cells. The results indicate that GNPs are excellent candidates as reinforcements in Mg matrices for the manufacture of biodegradable Mg-based composite implants. GNP addition improved the mechanical properties of Mg via synergetic strengthening modes. Moreover, retaining the structural integrity of GNPs during PM processing improved the ductility, compressive strength, and corrosion resistance of the Mg-GNP composites as compared to monolithic Mg. Cytotoxicity assessments did not reveal any significant toxicity with the addition of GNPs to Mg matrices. This study demonstrates that Mg-xGNPs with x < 0.3 wt.%, may constitute novel biodegradable implant materials for load-bearing applications.

Keywords: magnesium-graphene composites, strengthening mechanisms, In vitro cytotoxicity, biocorrosion

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Authors: Po-Hui Yang, Jing-Min Chen, Po-Yu Kuo, Chia-Chun Wu

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This paper proposed a high resolution Vernier Delay Line (VDL) measurement circuit with coarse and fine detection mechanism, which improved the trade-off problem between high resolution and less delay cells in traditional VDL circuits. And the measuring time of proposed measurement circuit is also under the high resolution requests. At first, the testing range of input signal which proposed high resolution delay line is detected by coarse detection VDL. Moreover, the delayed input signal is transmitted to fine detection VDL for measuring value with better accuracy. This paper is implemented at 0.18μm process, operating frequency is 100 MHz, and the resolution achieved 2.0 ps with only 16-stage delay cells. The test range is 170ps wide, and 17% stages saved compare with traditional single delay line circuit.

Keywords: vernier delay line, D-type flip-flop, DFF, metastable phenomenon

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Authors: S. K. M. Nzaba, H. H. Nyoni, B. Ntsendwana, B. B. Mamba, A. T. Kuvarega

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Azo dye effluents, released into water bodies are not only toxic to the ecosystem but also pose a serious impact on human health due to the carcinogenic and mutagenic effects of the compounds present in the dye discharge. Conventional water treatment methods such as adsorption, flocculation/coagulation and biological processes are not effective in completely removing most of the dyes and their natural degradation by-products. Advanced oxidation processes (AOPs) have proven to be effective technologies for complete mineralization of these recalcitrant pollutants. Therefore, there is a need for new technology that can solve the problem. Thus, this study examined the photocatalytic degradation of an azo dye brilliant black (BB) using non-metal/metal codoped TiO₂. N, Pt co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine-terminated polyamidoamine dendrimer generation 0 (PAMAM G0), amine-terminated polyamidoamine dendrimer generation 1 ( PAMAM G1) and hyperbranched polyethyleneimine (HPEI) as templates and source of nitrogen. Structural, morphological, and textural properties were evaluated using scanning electron microscopy coupled to energy dispersive X-ray spectroscopy (SEM/EDX), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), Fourier- transform infrared (FTIR), Raman spectroscopy (RS), photoluminescence (PL) and ultra-violet /visible spectroscopy (UV-Vis). The synthesized photocatalysts exhibited lower band gap energies as compared to the Degussa P-25 revealing a red shift in band gap towards the visible light absorption region. Photocatalytic activity of N, Pt co-doped TiO₂ was measured by the reaction of photocatalytic degradation of brilliant black (BB) dye. The N, metal codoped TiO₂ containing 0.5 wt. % of the metal consisted mainly of the anatase phase as confirmed by XRD results of all three samples, with a particle size range of 13–30 nm. The particles were largely spherical and shifted the absorption edge well into the visible region. Band gap reduction was more pronounced for the N, Pt HPEI (Pt 0.5 wt. %) codoped TiO₂ compared to PAMAM G0 and PAMAM G1. Consequently, codoping led to an enhancement in the photocatalytic activity of the materials for the degradation of brilliant black (BB).

Keywords: codoped TiO₂, dendrimer, photodegradation, wastewater

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Authors: Radka Králová, Libor Kvítek, Václav Ranc, Aleš Panáček, Radek Zbořil

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Surface–Enhanced Raman Scattering (SERS) is an optical spectroscopic technique with very good potential for sensitive detection of substances. In this research, active substrates with high enhancement were provided. Novel silver particles (nanostructures) with high roughened, flower–like morphology were prepared by reduction of cation complex [Ag(NH3)2]+ in presence of sodium borohydride as reducing agent and stabilized polyacrylic acid. The products were characterized by UV/VIS absorption spectrophotometry. Special shapes of silver particles were determined by scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM). Dispersions of this particle were put on fixed substrate to producing suitable layer for SERS. Adenine was applied as basic substance whose effect of enhancement on the layer of silver nanostructures was studied. By comparison with our work, the important influence of stabilizers, polyacrylic acid with various molecular weight and concentration, on the transfer of particles and formation of new structure was confirmed.

Keywords: metals, nanostructures, chemical reduction, Raman spectroscopy, optical properties

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Authors: Seyed Mahdi Rafiaei

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In this investigation, red emitting Eu³⁺ doped YVO₄ nano-phosphors have been synthesized via the facile combustion method using isobutyl nitrite and urea fuels, individually. Field-emission scanning electron microscope (FE-SEM) images, high resolution transmission electron microscope (TEM) images and X-ray diffraction (XRD) spectra reveal that the mentioned fuels can be used successfully to synthesis YVO₄: Eu³⁺ nano-particles. Interestingly, the fuels have a large effect on the size and morphology of nano-phosphors as well as luminescence properties. Noteworthy the use of isobutyl nitrite provides an average particle size of 65 nm, while the employment of urea, results in the formation of larger particles and also provides higher photoluminescence emission intensity. The improved luminescence performance is attributed to the condition of chemical reaction via the combustion synthesis and the size of synthesized phosphors.

Keywords: phosphors, combustion, fuels, luminescence, nanostructure

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Authors: Lise Paule Labéjof, Raíza Sales Pereira Bizerra, Galileu Barbosa Costa, Thaísa Barros dos Santos

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Since the beginning of the microscopy, improving the image quality has always been a concern of its users. Especially for transmission electron microscopy (TEM), the problem is even more important due to the complexity of the sample preparation technique and the many variables that can affect the conservation of structures, proper operation of the equipment used and then the quality of the images obtained. Animal tissues being transparent it is necessary to apply a contrast agent in order to identify the elements of their ultrastructural morphology. Several methods of contrastation of tissues for TEM imaging have already been developed. The most used are the “in block” contrastation and “in situ” contrastation. This report presents an alternative technique of application of contrast agent in vivo, i.e. before sampling. By this new method the electromicrographies of the tissue sections have better contrast compared to that in situ and present no artefact of precipitation of contrast agent. Another advantage is that a small amount of contrast is needed to get a good result given that most of them are expensive and extremely toxic.

Keywords: image quality, microscopy research, staining technique, ultra thin section

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Authors: W. Handoko, F. Pahlevani, V. Sahajwalla

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Dual-phase high carbon steels (DHCS) are commonly known for their improved strength, hardness, and abrasive resistance properties due to co-presence of retained austenite and martensite at the same time. Retained austenite is a meta-stable phase at room temperature, and stability of this phase governs the response of DHCS at different conditions. This research paper studies the effect of RA stability on corrosion behaviour of high carbon steels after they have been immersed into 1.0 M NaCl solution for various times. For this purpose, two different steels with different RA stabilities have been investigated. The surface morphology of the samples before and after corrosion attack was observed by secondary electron microscopy (SEM) and atomic force microscopy (AFM), along with the weight loss and Vickers hardness analysis. Microstructural investigations proved the preferential attack to retained austenite phase during corrosion. Hence, increase in the stability of retained austenite in dual-phase steels led to decreasing the weight loss rate.

Keywords: high carbon steel, austenite stability, atomic force microscopy, corrosion

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Authors: J. Marx, D. Smazna, R. Adelung, B. Fiedler

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Aerographite is a 3D interconnected carbon foam. Its tetrapodal morphology is based on the zinc oxide (ZnO) template structure, which is replicated in the chemical vapour deposition (CVD) into a hollow carbon structure. This replication process is analyzed in ex-situ studies via interrupted synthesis and the observation of the reaction progress by using scanning electron (SEM), transmission electron microscopy (TEM) and Raman spectroscopy techniques. Based on the epitaxial growth process, with a layer-by-layer growth behaviour of the wall thickness or number of layers and the catalytical graphitization of the deposited amorphous carbon into graphitic carbon by zinc, a growth model is created. The properties of aerographite, such as the electrical conductivity is dependent on the graphitization and number of layer (wall thickness). Wall thicknesses between 3 nm and 22 nm are achieved by a controlled stepwise reduction of the synthesis time on the basis of the developed growth model, and by a further thermal treatment at 1800 °C the graphitization of the presented carbon foam is modified. The variation of the wall thickness leads to an optimum defect density (ID/IG ratio) and the graphitization to an improvement in the electrical conductivity. Furthermore, a metallic conducting behaviour of untreated and 1800 °C treated aerographite can be observed. Due to these structural and defective modifications, a fundamental structural-property equation for the description of their influences on the electrical conductivity is developed.

Keywords: electrical conductivity, electron microscopy (SEM/TEM), graphitization, wall thickness

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Authors: Djamil Guettiche, Ahmed Mekki, Tighilt Fatma-Zohra, Rachid Mahmoud

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The aim of this study was to synthesize and characterize conducting polymer composites of polypyrrole and graphene, including pristine and surface-treated graphene (PPy/GO, PPy/rGO, and PPy/rGO-ArCOOH), for use as sensitive elements in a homemade chemiresistive module for on-line detection of nitrogen oxides vapors. The chemiresistive module was prepared, characterized, and evaluated for performance. Structural and morphological characterizations of the composite were carried out using FTIR, Raman spectroscopy, and XRD analyses. After exposure to NO and NO₂ gases in both static and dynamic modes, the sensitivity, selectivity, limit of detection, and response time of the sensor were determined at ambient temperature. The resulting sensor showed high sensitivity, selectivity, and reversibility, with a low limit of detection of 1 ppm. A composite of polypyrrole and graphene functionalized with aryl 4-carboxy benzene diazonium salt was synthesized and characterized using FTIR, scanning electron microscopy, transmission electron microscopy, UV-visible, and X-ray diffraction. The PPy-rGOArCOOH composite exhibited a good electrical resistance response to NO₂ at room temperature and showed enhanced NO₂-sensing properties compared to PPy-rGO thin films. The selectivity and stability of the NO₂ sensor based on the PPy/rGO-ArCOOH nanocomposite were also investigated.

Keywords: conducting polymers, surface treated graphene, diazonium salt, polypyrrole, Nitrogen oxide sensing

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Authors: Mohit Kalra, Varun S., Mayuri Gandhi

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CeF3 nanophosphors has been extensively investigated in the recent years for lighting and numerous bio-applications. Down conversion emissions in CeF3:Eu3+/Tb3+ phosphors were studied with the aim of obtaining a white light emitting composition, by a simple co-precipitation method. The material was characterized by X-ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HR-TEM), Fourier Transform Infrared Spectroscopy (FT-IR) and Photoluminescence (PL). Uniformly distributed nanoparticles were obtained with an average particle size 8-10 nm. Different doping concentrations were performed and fluorescence study was carried out to optimize the dopants concentration for maximum luminescence intensity. The steady state and time resolved luminescence studies confirmed efficient energy transfer from the host to activator ions. Different concentrations of Tb 3+, Eu 3+ were doped to achieve a white light emitting phosphor for UV-based Light Emitting Diodes (LEDs). The nanoparticles showed characteristic emission of respective dopants (Eu 3+, Tb3+) when excited at the 4f→5d transition of Ce3+. The chromaticity coordinates for these samples were calculated and the CeF3 doped with Eu 3+ and Tb3+ gave an emission very close to white light. These materials may find its applications in optoelectronics and various bio applications.

Keywords: white light down-conversion, nanophosphors, LEDs, rare earth, cerium fluoride, lanthanides

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

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

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

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Authors: Seyedamirreza Shamsdini, Mohsen Mohammadi

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In this research, 18Ni-300 maraging steel powder particles are investigated by studying particle size distribution along with their morphology and grain structure. The powder analysis shows mostly spherical morphologies with cellular structures. A laser-based additive manufacturing process, selective laser melting (SLM) is used to produce samples for further investigation of mechanical properties and microstructure. Several uniaxial tensile tests are performed on the as-built parts to evaluate the mechanical properties. The macroscopic properties, as well as microscopic studies, are then investigated on the printed parts. Hardness measurements, as well as porosity levels, are measured for each sample and are correlated with microstructures through electron microscopy techniques such as Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The grain structure is studied for the as-printed specimens and compared to the powder particle microstructure. The cellular structure of the printed samples is observed to have dendritic forms with dendrite width dimensions similar to the powder particle cells. The process parameter is changed, and the study is performed for different powder layer thickness, and the resultant mechanical properties and grain structure are shown to be similar. A phase study is conducted both on the powder and the printed samples using X-Ray Diffraction (XRD) techniques, and the austenite phase is observed to at first decrease due to the manufacturing process and again during the uniaxial tensile deformation. The martensitic structure is formed in the first stage based on the heating cycles of the manufacturing process and the remaining austenite is shown to be transformed to martensite due to different deformation mechanisms.

Keywords: additive manufacturing, maraging steel, mechanical properties, microstructure

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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: Hubert Beisch, Janik Marx, Svenja Garlof, Roman Shvets, Ivan Grygorchak, Andriy Kityk, Bodo Fiedler

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Three-dimensional carbon materials can be used as electrode materials for energy storage systems such as batteries and supercapacitors. Fast charging and discharging times are realizable without reducing the performance due to aging processes. Furthermore high specific surface area (SSA) of three-dimensional carbon structures leads to high specific capacities. One newly developed carbon foam is Globugraphite. This interconnected globular carbon morphology with statistically distributed hierarchical pores is manufactured by a chemical vapor deposition (CVD) process from ceramic templates resulting from a sintering process. Via scanning electron (SEM) and transmission electron microscopy (TEM), the morphology is characterized. Moreover, the SSA was measured by the Brunauer–Emmett–Teller (BET) theory. Measurements of Globugraphite in an organic and inorganic electrolyte show high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. A comparison of the specific values is summarized in a Ragone diagram. Energy densities up to 48 Wh/kg and power densities to 833 W/kg could be achieved for an SSA from 376 m²/g to 859 m²/g. For organic electrolyte, a specific capacity of 100 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, carbon foam, CVD process, electrochemical cell, Ragone diagram, SEM, TEM

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Authors: Hatem Diaf, Patrice Melinon, Antonio Pereira, Bernard Moine, Nicholas Blanchard, Florent Bourquard, Florence Garrelie, Christophe Donnet

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Glassy carbon exhibits excellent biological compatibility with live tissues meaning it has high potential for applications in life science. Moreover, glassy carbon has interesting properties including 'high temperature resistance', hardness, low density, low electrical resistance, low friction, and low thermal resistance. The structure of glassy carbon has long been a subject of debate. It is now admitted that glassy carbon is 100% sp2. This term is a little bit confusing as long sp2 hybridization defined from quantum chemistry is related to both properties: threefold configuration and pi bonding (parallel pz orbitals). Using plasma laser deposition of carbon clusters combined with pulsed nano/femto laser annealing, we are able to synthesize thin films of glassy carbon of good quality (probed by G band/ D disorder band ratio in Raman spectroscopy) without thermal post annealing. A careful inspecting of Raman signal, plasmon losses and structure performed by HRTEM (High Resolution Transmission Electron Microscopy) reveals that both properties (threefold and pi orbitals) cannot coexist together. The structure of the films is compared to models including schwarzites based from negatively curved surfaces at the opposite of onions or fullerene-like structures with positively curved surfaces. This study shows that a huge collection of porous carbon named vitreous carbon with different structures can coexist.

Keywords: glassy carbon, cluster deposition, coating, electronic structure

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Authors: Carlos Alberto Ríos-Reyes, Efraín Casadiego-Quintero

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We propose a generalized workflow for mineralogy investigation of unconventional reservoirs using multi-scale imaging and pore-scale analyses. This workflow can be used for the integral evaluation of these resources. The Cretaceous La Luna Formation´s mudstones in the Middle Magdalena Valley Basin (Colombia) inherently show a heterogeneous pore system with organic and inorganic pores. For this reason, it is necessary to carry out the integration of high resolution 2D images of mapping by conventional petrography, scanning electron microscopy and quantitative evaluation of minerals by scanning electron microscopy to describe their organic and inorganic porosity to understand the transport mechanism through pores. The analyzed rocks show several pore types, including interparticle pores, organoporosity, intraparticle pores, intraparticle pores, and microchannels and/or microfractures. The existence of interconnected pores in pore system of these rocks promotes effective pathways for primary gas migration and storage space for residual hydrocarbons in mudstones, which is very useful in this type of gas reservoirs. It is crucial to understand not only the porous system of these rocks and their mineralogy but also to project the gas flow in order to design the appropriate strategies for the stimulation of unconventional reservoirs. Keywords: mudstones; La Luna Formation; gas storage; migration; hydrocarbon.

Keywords: mudstones, La luna formation, gas storage, migration, hydrocarbon

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Authors: Alak Kumar Patra, Nilanjan Mitra

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Interface fracture toughness of glass-epoxy (G/E) PVC core sandwich composite with and without MWCNT has been investigated through experimental methods. Results demonstrate an improvement in interface fracture toughness values (GC) of samples with a certain percentages of MWCNT. In addition, dispersion of MWCNT in epoxy resin through sonication followed by mixing of hardener and vacuum assisted resin transfer method (VARTM) used in this study is an easy and cost effective methodology in comparison to previously adopted other methods limited to laminated composites. The study also identifies the optimum weight percentage of MWCNT addition in the resin system for maximum performance gain in interfacial fracture toughness. The results are supported by high resolution transmission electron microscope (HRTEM) analysis and fracture micrograph of field emission scanning electron microscope (FESEM) investigation.

Keywords: carbon nanotube, foam, glass-epoxy, interfacial fracture, sandwich composite

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

Abstract:

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: Jung-Hwan Oh, Rajesh Kumar, Il-Kwon Oh

Abstract:

Porous graphene has extensive potential applications in variety of fields such as hydrogen storage, CO oxidation, gas separation, supercapacitors, fuel cells, nanoelectronics, oil adsorption, and so on. However, the generation of some carbon atoms vacancies for precise small holes have been not extensively studied to prevent the agglomerates of graphene sheets and to obtain porous graphene with high surface area. Recently, many research efforts have been presented to develop physical and chemical synthetic approaches for porous graphene. But physical method has very high cost of manufacture and chemical method consumes so many hours for porous graphene. Herein, we propose a porous graphene contained holes with atomic scale precision by embedding metal nano-particles through microwave irradiation for hydrogen storage and CO oxidation multi- functionalities. This proposed synthetic method is appropriate for fast and convenient production of three dimensional nanostructures, which have nanoholes on the graphene surface in consequence of microwave irradiation. The metal nanoparticles are dispersed quickly on the graphene surface and generated uniform nanoholes on the graphene nanosheets. The morphological and structural characterization of the porous graphene were examined by scanning electron microscopy (SEM), transmission scanning electron microscopy (TEM) and RAMAN spectroscopy, respectively. The metal nanoparticle-embedded porous graphene exhibits a microporous volume of 2.586cm3g-1 with an average pore radius of 0.75 nm. HR-TEM analysis was carried out to further characterize the microstructures. By investigating the RAMAN spectra, we can understand the structural changes of graphene. The results of this work demonstrate a possibility to produce a new class of porous graphene. Furthermore, the newly acquired knowledge for the diffusion into graphene can provide useful guidance for the development of the growth of nanostructure.

Keywords: CO oxidation, hydrogen storage, nanocomposites, porous graphene

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Authors: Rimzhim Gupta, Bhanupriya Boruah, Jayant M. Modak, Giridhar Madras

Abstract:

Microbial contamination is one of the major concerns in the field of water treatment. AOP (advanced oxidation processes) is well-established method to resolve the issue of removal of contaminants in water. A Z-scheme composite g-C₃N₄/CuWO₄ was synthesized by sol-gel method for the photocatalytic inactivation of a mixed population of Gram-positive bacteria (S. aureus) and Gram-negative bacteria (E. coli). The photoinactivation was observed for different types of bacteria in the same medium together and individually in the absence of the nutrients. The lattice structures and phase purities were determined by X-ray diffraction. For morphological and topographical features, scanning electron microscopy and transmission electron microscopy analyses were carried out. The band edges of the semiconductor (valence band and conduction band) were determined by ultraviolet photoelectron microscopy. The lifetime of the charge carriers and band gap of the semiconductors were determined by time resolved florescence spectroscopy and diffused reflectance spectroscopy, respectively. The effect of weight ratio of C₃N₄ and CuWO₄ was observed by performing photocatalytic experiments. To investigate the exact mechanism and major responsible radicals for photocatalysis, scavenger studies were performed. The rate constants and order of the inactivation reactions were obtained by power law kinetics. For E. coli and S. aureus, the order of reaction and rate constants are 1.15, 0.9 and 1.39 ± 0.03 (CFU/mL)⁻⁰.¹⁵ h⁻¹, 47.95 ± 1.2 (CFU/mL)⁰.¹ h⁻¹, respectively.

Keywords: z-scheme, E. coli, S. aureus, sol-gel

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Authors: Lucja Rodzik, Joanna Lewandowska-Lancucka, Michal Szuwarzynski, Krzysztof Szczubialka, Maria Nowakowska

Abstract:

The analysis of nucleobases is of great importance for bioscience since their abnormal concentration in body fluids suggests the deficiency and mutation of the immune system, and it is considered to be an important parameter for diagnosis of various diseases. The presented conjugate meets the need for development of the effective, selective and highly sensitive sensor for nucleobase/nucleoside detection. The novel, highly fluorescent cadmium telluride quantum dots (CdTe QDs) functionalized with thymine and stabilized with thioglycolic acid (TGA) conjugates has been developed and thoroughly characterized. Successful formation of the material was confirmed by elemental analysis, and UV–Vis fluorescence and FTIR spectroscopies. The crystalline structure of the obtained product was characterized with X-ray diffraction (XRD) method. The composition of CdTe QDs and their thymine conjugate was also examined using X-ray photoelectron spectroscopy (XPS). The size of the CdTe-thymine was 3-6 nm as demonstrated using atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM) imaging. The plasmon resonance fluorescence band at 540 nm on excitation at 351 nm was observed for these nanoparticles. The intensity of this band increased with the increase in the amount of conjugated thymine with no shift in its position. Based on the fluorescence measurements, it was found that the CdTe-thymine conjugate interacted efficiently and selectively not only with adenine, a nucleobase complementary to thymine, but also with nucleosides and adenine-containing modified nucleosides, i.e., 5′-deoxy-5′-(methylthio)adenosine (MTA) and 2’-O-methyladenosine, the urinary tumor markers which allow monitoring of the disease progression. The applicability of the CdTe-thymine sensor for the real sample analysis was also investigated in simulated urine conditions. High sensitivity and selectivity of CdTe-thymine fluorescence towards adenine, adenosine and modified adenosine suggest that obtained conjugate can be potentially useful for development of the biosensor for complementary nucleobase/nucleoside detection.

Keywords: CdTe quantum dots, conjugate, sensor, thymine

Procedia PDF Downloads 377