Search results for: scanning electron microscopic analysis

Authors: Eyyup Murat Karakurt, Yan Huang, Mehmet Kaya, Huseyin Demirtas

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In this study, the effect of the porosity effect of Ti-20Zr alloy produced by powder metallurgy as a biomaterial was investigated experimentally. The Ti based alloys (Ti-20%Zr (at.) were produced under 300 MPa, for 6 h at 1200 °C. Afterward, the microstructure of the Ti-based alloys was analyzed by optical analysis, scanning electron microscopy, energy dispersive spectrometry. Moreover, compression tests were applied to determine the mechanical behaviour of samples. As a result, highly porous Ti-20Zr alloys exhibited an elastic modulus close to human bone. The results later were compared theoretically and experimentally.

Keywords: porosity effect, Ti based alloys, elastic modulus, compression test

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

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

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

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Authors: Malihe Moeinin, Robert Hill, Ferranti Wong

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Background: A white spot lesion (WSL) is defined as subsurface enamel porosity from carious demineralisation on the smooth surfaces of the tooth. It appears as a milky white opacity. Lesions shown an apparently intact surface layer, followed underneath by the more porous lesion body. The small pores within the body of the lesion act as diffusion pathway for both acids and minerals, so allowing the demineralisation of enamel to occur at the advancing front of the lesion. Objectives: The objective is to mapthe porosity and its size on WSL with Focused Ion Bean- Scanning Electron Microscopy (FIB-SEM) Method: The basic method used for FIB-SEM consisted of depositing a one micron thick layer of platinum over 25μmx 25μm of the interest region of enamel. Then, making a rough cut (25μmx 5μmx 20μm) with 3nA current and 30Kv was applied with the help of drift suppression (DS), using a standard “cross-sectional” cutting pattern, which ended at the front of the deposited platinum layer. Two adjacent areas (25μmx 5μmx 20μm) on the both sides of the platinum layer were milled under the same conditions. Subsequent, cleaning cross-sections were applied to polish the sub-surface edge of interest running perpendicular to the surface. The "slice and view" was carried out overnight for milling almost 700 slices with 2Kv and 4nA and taking backscattered (BS) images. Then, images were imported into imageJ and analysed. Results: The prism structure is clearly apparent on FIB-SEM slices of WSL with the dissolution of prism boundaries as well as internal porosity within the prism itself. Porosity scales roughly 100-400nm, which is comparable to the light wavelength (500nm). Conclusion: FIB-SEM is useful to characterize the porosity of WSL and it clearly shows the difference between WSL and normal enamel.

Keywords: white spot lesion, FIB-SEM, enamel porosity, porosity

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Authors: Renu Kumari, Jyotsna Dutta Majumdar

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In the present study, composite coating consisting of hydroxyapatite (HA) + 50 wt% TiO2 has been developed on Ti-6Al-4V substrate by plasma spray deposition technique. Followed by plasma spray deposition, detailed surface roughness and microstructural characterization were carried out by using optical profilometer and scanning electron microscopy (SEM), respectively. The composition and phase analysis were carried out by energy-dispersive X-ray spectroscopy analysis, and X-ray diffraction (XRD) technique, respectively. The bio-activity behavior of the uncoated and coated samples was also compared by dipping test in Hank’s solution. The average surface roughness of the coating was 10 µm (as compared to 0.5 µm of as-received Ti-6Al-4V substrate) with the presence of porosities. The microstructure of the coating was found to be continuous with the presence of solidified splats. A detailed XRD analysis shows phase transformation of TiO2 from anatase to rutile, decomposition of hydroxyapatite, and formation of CaTiO3 phase. Standard dipping test confirmed a faster kinetics of deposition of calcium phosphate in the coated HA+50% wt.% TiO2 surface as compared to the as-received substrate.

Keywords: titanium, plasma spraying, microstructure, bio-activity, TiO2, hydroxyapatite

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Authors: E. Moroydor Derun, P. Gurses, M. Yildirim, A. S. Kipcak, T. Ibroska, S. Piskin

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Due to their strong mechanical and thermal properties magnesium borates have a wide usage area such as ceramic industry, detergent production, friction reducing additive and grease production. In this study, microwave synthesis of magnesium borates from MgCl2.6H2O (Magnesium chloride hexahydrate), MgO (Magnesium oxide) and H3BO3 (Boric acid) for different reaction times is researched. X-ray Diffraction (XRD) and Fourier Transform Infrared (FT-IR) Spectroscopy are used to find out how the reaction time sways on the products. The superficial properties are investigated with Scanning Electron Microscopy (SEM). According to XRD analysis, the synthesized compounds are 00-041-1407 pdf coded Shabinite (Mg5(BO3)4Cl2(OH)5.4(H2O)) and 01-073-2158 pdf coded Karlite (Mg7(BO3)3(OH,Cl)5).

Keywords: magnesium borate, microwave synthesis, XRD, SEM

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Authors: Krasimir I. Ivanov, Penka S. Zapryanova, Stefan V. Krustev, Violina R. Angelova

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Three commonly used digestion methods (dry ashing, acid digestion, and microwave digestion) in different variants were compared for digestion of tobacco leaves. Three main macroelements (K, Ca and Mg) were analysed using AAS Spectrometer Spectra АА 220, Varian, Australia. The accuracy and precision of the measurements were evaluated by using Polish reference material CTR-VTL-2 (Virginia tobacco leaves). To elucidate the problems with elemental recovery X-Ray and SEM–EDS analysis of all residues after digestion were performed. The X-ray investigation showed a formation of KClO₄ when HClO4 was used as a part of the acids mixture. The use of HF at Ca and Mg determination led to the formation of CaF₂ and MgF₂. The results were confirmed by energy dispersive X-ray microanalysis. SPSS program for Windows was used for statistical data processing.

Keywords: digestion methods, plant tissue, determination of macroelements, K, Ca, Mg

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Authors: Anjela Koblischka-Veneva, Michael Koblischka

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In this contribution, the transmission-Kikuchi diffrac-tion (TKD, or sometimes called t-EBSD) is applied to bulk, melt-grown YBa2Cu3O7 (YBCO) superconductors prepared by the MTMG (melt-textured melt-grown) technique and the infiltration (IG) growth technique. TEM slices required for the analysis were prepared by means of focused ion-beam (FIB) milling using mechanically polished sample surfaces, which enable a proper selection of the in-teresting regions for investigations. The required optical transparency was reached by an additional polishing step of the resulting surfaces using FIB-Ga-ion and Ar-ion milling. The improved spatial resolution of TKD enabled the investigation of the tiny Y2BaCuO5 (Y-211) particles having a diameter of about 50-100 nm embedded within the YBCO matrix and of other added secondary phase particles. With the TKD technique, the microstructural properties of the YBCO matrix are studied in detail. It is observed that the matrix shows effects of stress/strain, depending on the size and distribution of the embedded particles, which are important for providing additional flux pinning centers in such superconducting bulk samples. Using the Kernel average misorientation (KAM) maps, the strain induced in the superconducting matrix around the particles, which increases the flux pinning effectivity, can be clearly revealed. This type of analysis of the EBSD/TKD data is, therefore, also important for other material systems, where nanoparticles are embedded in a matrix.

Keywords: electron backscatter Diffraction, transmission Kikuchi diffraction, SEM, YBCO, microstructure, nanoparticles

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Authors: Chiun-C.R. Wang, Po-Wen Yen, Chien-Chun Huang

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Banana is produced in large quantities in tropical and subtropical areas. Banana is one of the important fruits which constitute a valuable source of energy, vitamins and minerals. The ripening and maturity standards of banana vary from country to country depending on the expected shelf life of market. The compositions of bananas change dramatically during ethylene-induced ripening that are categorized as nutritive values and commercial utilization. Nevertheless, there is few study reporting the changes of physicochemical properties of banana starch during ethylene-induced ripening of green banana. The objectives of this study were to investigate the changes of chemical composition and enzyme activity of banana and physicochemical properties of banana starch during ethylene-induced ripening. Green bananas were harvested and ripened by ethylene gas at low temperature (15℃) for seven stages. At each stage, banana was sliced and freeze-dried for banana flour preparation. The changes of total starch, resistant starch, chemical compositions, physicochemical properties, activity of amylase, polyphenolic oxidase (PPO) and phenylalanine ammonia lyase (PAL) of banana were analyzed each stage during ripening. The banana starch was isolated and analyzed for gelatinization properties, pasting properties and microscopic appearance each stage of ripening. The results indicated that the highest total starch and resistant starch content of green banana were 76.2% and 34.6%, respectively at the harvest stage. Both total starch and resistant starch content were significantly declined to 25.3% and 8.8%, respectively at the seventh stage. Soluble sugars content of banana increased from 1.21% at harvest stage to 37.72% at seventh stage during ethylene-induced ripening. Swelling power of banana flour decreased with the progress of ripening stage, but solubility increased. These results strongly related with the decreases of starch content of banana flour during ethylene-induced ripening. Both water insoluble and alcohol insoluble solids of banana flour decreased with the progress of ripening stage. Both activity of PPO and PAL increased, but the total free phenolics content decreased, with the increases of ripening stages. As ripening stage extended, the gelatinization enthalpy of banana starch significantly decreased from 15.31 J/g at the harvest stage to 10.55 J/g at the seventh stage. The peak viscosity and setback increased with the progress of ripening stages in the pasting properties of banana starch. The highest final viscosity, 5701 RVU, of banana starch slurry was found at the seventh stage. The scanning electron micrograph of banana starch showed the shapes of banana starch appeared to be round and elongated forms, ranging in 10-50 μm at the harvest stage. As the banana closed to ripe status, some parallel striations were observed on the surface of banana starch granular which could be caused by enzyme reaction during ripening. These results inferred that the highest resistant starch was found in the green banana at the harvest stage could be considered as a potential application of healthy foods. The changes of chemical composition and physicochemical properties of banana could be caused by the hydrolysis of enzymes during the ethylene-induced ripening treatment.

Keywords: ethylene-induced ripening, banana starch, resistant starch, soluble sugars, physicochemical properties, gelatinization enthalpy, pasting characteristics, microscopic appearance

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Authors: Nihit Madireddi, P. A. Mahanwar

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We have aimed to produce a self-cleaning transparent polymer coating with polyurethane (PU) matrix as the latter is highly solvent, chemical and weather resistant having good mechanical properties. Nano-silica modified by 1H, 1H, 2H, 2H-perflurooctyltriethoxysilane was incorporated into the PU matrix for attaining self-cleaning ability through hydrophobicity. The modification was confirmed by particle size analysis and scanning electron microscopy (SEM). Thermo-gravimetric (TGA) studies were carried to ascertain the grafting of silane onto the silica. Several coating formulations were prepared by varying the silica loading content and compared to a commercial equivalent. The effect of dispersion and the morphology of the coated films were assessed by SEM analysis. All coating standardized tests like solvent resistance, adhesion, flexibility, acid, alkali, gloss etc. have been performed as per ASTM standards. Water contact angle studies were conducted to analyze the hydrophobic character of the coating. In addition, the coatings were also subjected to salt spray and accelerated weather testing to analyze the durability of the coating.

Keywords: FAS, nano-silica, PU clear coat, self-cleaning

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Authors: Md. Hafezur Rahaman, Md. Sagor Hosen, Md. Abdul Gafur, Rasel Habib

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This research is a systematic study of effects of poly(D-lactic acid) (PDLA) on the properties of poly(L-lactic acid)(PLLA)/microcrystalline cellulose (MCC)/PDLA blends by stereo complex crystallization. Blends were prepared with constant percentage of (3 percent) MCC and different percentage of PDLA by solution casting methods. These blends were characterized by Fourier Transform Infrared Spectroscopy (FTIR) for the confirmation of blends compatibility, Wide-Angle X-ray Scattering (WAXS) and scanning electron microscope (SEM) for the analysis of morphology, thermo-gravimetric analysis (TGA) and differential thermal analysis (DTA) for thermal properties measurement. FTIR Analysis results confirm no new characteristic absorption peaks appeared in the spectrum instead shifting of peaks due to hydrogen bonding help to have compatibility of blends component. Development of three new peaks from XRD analysis indicates strongly the formation of stereo complex crystallinity in the PLLA structure with the addition of PDLA. TGA and DTG results indicate that PDLA can improve the heat resistivity of the PLLA/MCC blends by increasing its degradation temperature. Comparison of DTA peaks also ensure developed thermal properties. Image of SEM shows the improvement of surface morphology.

Keywords: microcrystalline cellulose, poly(l-lactic acid), stereocomplex crystallization, thermal stability

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Authors: R. H. Bari

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The nanostructured thin films of CdSnO3 are sensitive to change in their environment. CdSnO3 is successfully used as gas sensor due to the dependence of the electrical conductivity on the ambient gas composition. Nanostructured CdSnO3 thin films of different substrate temperature (300 0C, 350 0C, 400 0C and 450 0C) were deposited onto heated glass substrate by simple spray pyrolysis (SP) technique. Sensing elements of nanostructured CdSnO3 were annealed at 500 0C for 1 hrs. Characterization includes a different analytical technique such as, X-ray diffractogram (XRD), energy dispersive X-ray analysis (EDAX), and Field emission scanning electron microscope (FE-SEM). The average grain size observed from XRD and FF-SEM was found to be less than 18.36 and 23 nm respectively. The films sprayed at substrate temperature for 400 0C was observed to be most sensitive (S = 530) to SO2 for 500 ppm at 300 0C. The response and recovery time is 4 sec, 8 sec respectively.

Keywords: nanostructured CdSnO3, spray pyrolysis, SO2 gas sensing, quick response

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Authors: Wenliang Song, Yu Zhang, Hua Jin, Il Kim

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The self-assembly of the polypeptide (PP) into well-defined structures at different length scales is both biomimetic relevant and fundamentally interesting. Although there are various reports of nanostructures fabricated by the self-assembly of various PPs, directed self-assembly of PP into three-dimensional (3D) hierarchical structure has proven to be difficult, despite their importance for biological applications. Herein, an efficient method has been developed through living polymerization of phenylalanine N-Carboxy anhydride (NCA) towards the linear and cyclic polyphenylalanine, and the new invented swelling methodology can form diverse hierarchical polypeptide crystals. The solvent-dependent self-assembly behaviors of these homopolymers were characterized by high-resolution imaging tools such as atomic force microscopy, transmission electron microscopy, scanning electron microscope. The linear and cyclic polypeptide formed 3D nano hierarchical shapes, such as a sphere, cubic, stratiform and hexagonal star in different solvents. Notably, a crystalline packing model was proposed to explain the formation of 3D nanostructures based on the various diffraction patterns, looking forward to give an insight for their dissimilar shape inflection during the self-assembly process.

Keywords: self-assembly, polypeptide, bio-polymer, crystalline polymer

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Authors: Jenny Radeva, Anke-Gundula Roth, Christian Goebbert, Robert Niestroj-Pahl, Lars Daehne, Axel Wolfram, Juergen WIese

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The presented investigation studies the correlation between the process parameters of Layer-by-Layer (LbL) coatings and properties of the produced hybrid membranes for water treatment. The coating of alumina ceramic support membrane with polyelectrolyte multilayers on top results in hybrid membranes with increased fouling resistant behavior, high retention (up to 90%) of salt ions and various pharmaceuticals, selectivity to various organic molecules as known from LbL coated polyether sulfone membranes and the possibility of pH response control. Chosen polyelectrolytes were added to the support using the LbL-coating process. Parameters like the type of polyelectrolyte, ionic strength, and pH were varied in order to find the most suitable process conditions and to study how they influence the properties of the final product. The applied LbL-films was investigated in respect to its homogeneity and penetration depth. The analysis of the layer buildup was performed using fluorescence labeled polyelectrolyte molecules and Confocal Laser Scanning Microscopy as well as Scanning and Transmission Electron Microscopy. Furthermore, the influence of the coating parameters on the porosity, surface potential, retention, and permeability of the developed hybrid membranes were estimated. In conclusion, a comparison was drawn between the filtration performance of the uncoated alumina ceramic membrane and modified hybrid membranes.

Keywords: water treatment, membranes, ceramic membranes, hybrid membranes, layer-by-layer modification

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Authors: Chady El Hachem, Pan Ye, Kamilia Abahri, Rachid Bennacer

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Considered as a building construction material, and regarding its environmental benefits, wood fiber insulation is the material of interest in this work. The definition of adequate elementary representative volume that guarantees reliable understanding of the hygrothermal macroscopic phenomena is very critical. At the microscopic scale, when subjected to hygric solicitations, fibers undergo local dimensionless variations. It is therefore necessary to master this behavior, which affects the global response of the material. This study consists of an experimental procedure using the non-destructive method, X-ray tomography, followed by morphological post-processing analysis using ImageJ software. A refine investigation took place in order to identify the representative elementary volume and the sufficient resolution for accurate structural analysis. The second part of this work was to evaluate the microscopic hygric behavior of the studied material. Many parameters were taken into consideration, like the evolution of the fiber diameters, distribution along the sorption cycle and the porosity, and the water content evolution. In addition, heat transfer simulations based on the energy equation resolution were achieved on the real structure. Further, the problematic of representative elementary volume was elaborated for such heterogeneous material. Moreover, the material’s porosity and its fibers’ thicknesses show very big correlation with the water content. These results provide the literature with very good understanding of wood fiber insulation’s behavior.

Keywords: hygric behavior, morphological characterization, wood fiber insulation material, x-ray tomography

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Authors: Rajesh Bansal, Amit Raj Sharma, Vakil Singh

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The success and predictability of titanium implants for long durations are well established and there has been a tremendous increase in the popularity of implants among patients as well as clinicians over the last four decades. However, sometimes complications arise, which lead to the loss of the implant as well as the prosthesis. Fracture of dental implants is rare; however, at times, implants or abutment screws fracture and lead to many problems for the clinician and the patient. Possible causes of implant fracture include improper design, overload, fatigue and corrosion. Six retrieved fractured dental implants, with varying diameters and designs, were collected from time to time to examine by scanning electron microscope (SEM) to characterize fracture behavior and assess the mechanism of fracture. In this investigation, it was observed that fracture of the five dental implants occurred due to fatigue crack initiation and propagation from the thread roots.

Keywords: titanium, dental, implant, fracture, failure

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Authors: Afrah E. Mohammed, Mudawi M. Nour

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Environmentally friendly green synthesis of nanomaterial has a very significant part in nanotechnology. In the present research, the synthesis of silver nanoparticles (AgNPs) was established by treating silver ions with the aqueous extract of Calligonum comosum green shoots at room temperature. AgNPs formation was firstly detected by the colour change of mixed extract (plant extract and AgNO3). Further characterization was done by ultraviolet (UV)-Vis spectrophotometer, transmission electron microscopy (TEM), scanning electron microscopy (SEM), zeta potential and fourier transform infrared spectroscopy (FTIR). The peak values for UV-VIS- spectroscopy were in the range of 440 nm, TEM micrograph showed a spherical shape for the particles and zeta potential showed the formation of negative charged nanoparticles with an average size of about 105.8 nm. 1635.41 and 3249.83 cm−1 are the peaks detected from the FTIR analysis. In this study, biosynthesized silver nanoparticles mediated by C. comosum were tested for their antimycotic activity using a well diffusion method against fungal species; Aspergillus flavus, Penicillium sp, Fusarium oxysporum. Our findings indicated that biosynthesized AgNPs showed an efficient antimycotic activity against tested species. The antimycotic action of AgNPs varied according to different fungal species. Results confirmed the ability of C. comosum green shoot extract to act as an reducing and stabilizing agent during the synthesis of AgNPs.

Keywords: AGNPS, zeta potential, TEM, SEM

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Authors: Nuray Güy, Mahmut Özacar

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Semiconductor nanoparticles such as TiO₂ and ZnO as photocatalysts are very efficient catalysts for wastewater treatment by the chemical utilization of light energy, which is capable of converting the toxic and nonbiodegradable organic compounds into carbon dioxide and mineral acids. ZnO semiconductor has a wide bandgap energy of 3.37 eV and a relatively large exciton binding Energy (60 meV), thus can absorb only UV light with the wavelength equal to or less than 385 nm. It exhibits low efficiency under visible light illumination due to its wide band gap energy. In order to improve photocatalytic activity of ZnO under visible light, band gap of ZnO may be narrowed by doping such as N, C, S nonmetal ions and coupled two separate semiconductors possessing different energy levels for their corresponding conduction and valence bands. ZnS has a wider band gap (Eg=3.7 eV) than ZnO and generates electron–hole pairs by photoexcitation rapidly. In the present work, N doped ZnO/ZnS nano photocatalysts with visible-light response were synthesized by microwave-hydrothermal method using thiourea as N source. The prepared photocatalysts were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV–visible (UV–vis). The photocatalytic activities samples and undoped ZnO have been studied for the degradation of dye, and have also been compared with together.

Keywords: photocatalyst, synthesis, visible light, ZnO/ZnS

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Authors: Sonam Chorol, Sharvan Kumar, Pritam Mukhopadhyay

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In biology, supramolecular systems require the use of chemical fuels to stay in sustained nonequilibrium steady states termed dissipative self-assembly in contrast to synthetic self-assembly. Biomimicking these natural dynamic systems, some studies have demonstrated artificial self-assembly under nonequilibrium utilizing various forms of energies (fuel) such as chemical, redox, and pH. Naphthalene diimides (NDIs) are well-known organic molecules in supramolecular architectures with high electron affinity and have applications in controlled electron transfer (ET) reactions, etc. Herein, we report the endergonic ET from tetraphenylborate to highly electron-deficient phosphonium NDI²+ dication to generate NDI•+ radical. The formation of radicals was confirmed by UV-Vis-NIR absorption spectroscopy. Electron-donor and electron-acceptor energy levels were calculated from experimental electrochemistry and theoretical DFT analysis. The HOMO of the electron donor locates below the LUMO of the electro-acceptor. This indicates that electron transfer is endergonic (ΔE°ET = negative). The endergonic ET from NaBPh₄ to NDI²+ dication was achieved thermodynamically by the formation of coupled biphenyl product confirmed by GC-MS analysis. NDI molecule bearing octyl phosphonium at the core and H-bond forming imide moieties at the axial position forms a gel. The rheological properties of purified radical ion NDI⦁+ gels were evaluated. The atomic force microscopy studies reveal the formation of large branching-type networks with a maximum height of 70-80 nm. The endergonic ET from NaBPh₄ to NDI²+ dication was used to design the assembly and disassembly redox reaction cycle using reducing (NaBPh₄) and oxidizing agents (Br₂) as chemical fuels. A part of NaBPh₄ is used to drive assembly, while a fraction of the NaBPh₄ is dissipated by forming a useful product. The system goes back to the disassembled NDI²+ dication state with the addition of Br₂. We think bioinspired dissipative self-assembly is the best approach to developing future lifelike materials with autonomous behavior.

Keywords: Ionic-gel, redox-cycle, self-assembly, useful product

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Authors: Shahab Zomorodbakhsh, Hayron Nesa Motevasel

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Water soluble compoundes were attached to single-walled carbon nanotubes (SWNTs) to form water-soluble nano pigments. functionalized SWNTs were then characterized by Fourier Transform Infrared spectroscopy (FT-IR), Raman spectroscopy, UV analysis, Transmission electron microscopy (TEM)and defunctionalization test and Representative results concerning the solubility. The product can be dissolved in water and High-resolution transmission electron microscope images showed that the SWNTs were efficiently functionalized, thus the p-stacking interaction between aromatic rings and COOH of SWNTs was considered responsible for the high solubility and High transmission electron in singlewall nanotubes.

Keywords: functionalized CNTs, singlewalled carbon nanotubes, water soluble compoundes, nano pigments

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Authors: Ravi V. Joat, Pravin S. Bodke, Shradha S. Binani, S. S. Wasnik

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A phase diagram of the Ag2SO4 - CaSO4 (Silver sulphate – Calcium Sulphate) binaries system using conductivity, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis) data is constructed. The eutectic reaction (liquid -» a-Ag2SO4 + CaSO4) is observed at 10 mole% CaSO4 and 645°C. Room temperature solid solubility limit up to 5.27 mole % of Ca 2+ in Ag2SO4 is set using X-ray powder diffraction and scanning electron microscopy results. All compositions beyond this limit are two-phase mixtures below and above the transition temperature (≈ 416°C). The bulk conductivity, obtained following complex impedance spectroscopy, is found decreasing with increase in CaSO4 content. Amongst other binary compositions, the 80AgSO4-20CaSO4 gave improved sinterability/packing density.

Keywords: phase diagram, Ag2SO4-CaSO4 binaries system, conductivity, XRD, DTA

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Authors: L. Pu, C. Unluer

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MgO cements have the potential to sequester CO2 in construction products, and can be partial or complete replacement of PC in concrete. Construction block is a promising application for reactive MgO cements. Main advantages of blocks are: (i) suitability for sequestering CO2 due to their initially porous structure; (ii) lack of need for in-situ treatment as carbonation can take place during fabrication; and (iii) high potential for commercialization. Both strength gain and carbon sequestration of MgO cements depend on carbonation process. Fly ash and ground granulated blast-furnace slag (GGBS) are pozzolanic material and are proved to improve many of the performance characteristics of the concrete, such as strength, workability, permeability, durability and corrosion resistance. A very limited amount of work has been reported on the production of MgO blocks on a large scale so far. A much more extensive study, wherein blocks with different mix design is needed to verify the feasibility of commercial production. The changes in the performance of the samples were evaluated by compressive strength testing. The properties of the carbonation products were identified by X-ray diffraction (XRD) and scanning electron microscopy (SEM)/ field emission scanning electron microscopy (FESEM), and the degree of carbonation was obtained by thermogravimetric analysis (TGA), XRD and energy dispersive X-ray (EDX). The results of this study enabled the understanding the relationship between lab-scale samples and scale-up blocks based on their mechanical performance and microstructure. Results indicate that for both scaled-up and lab-scale samples, MgO samples always had the highest strength results, followed by MgO-fly ash samples and MgO-GGBS had relatively lowest strength. The lower strength of MgO with fly ash/GGBS samples at early stage is related to the relatively slow hydration process of pozzolanic materials. Lab-scale cubic samples were observed to have higher strength results than scaled-up samples. The large size of the scaled-up samples made it more difficult to let CO2 to reach inner part of the samples and less carbonation products formed. XRD, TGA and FESEM/EDX results indicate the existence of brucite and HMCs in MgO samples, M-S-H, hydrotalcite in the MgO-fly ash samples and C-S-H, hydrotalctie in the MgO-GGBS samples. Formation of hydration products (M-S-H, C-S-H, hydrotalcite) and carbonation products (hydromagnecite, dypingite) increased with curing duration, which is the reason of increasing strength. This study verifies the advantage of large-scale MgO blocks over common PC blocks and the feasibility of commercial production of MgO blocks.

Keywords: reactive MgO, fly ash, ground granulated blast-furnace slag, carbonation, CO₂

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Authors: Anjana Jain, S. Jayanth Kumar

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Polyvinylidene fluoride (PVDF) is a well-known material for remarkable mechanical properties, resistance to chemicals and superior ferroelectric performances. This endows PVDF the potential for application in supercapacitor devices. The dielectric properties of PVDF, however, are not very high. To improve the dielectric properties of Polyvinylidene fluoride (PVDF), Piezoelectric polymer nanocomposites are prepared without affecting the other useful properties of PVDF. Polyaniline (PANI) was chosen as a filler material to prepare the nanocomposites. PVDF-PANI nanocomposite films were prepared using solvent cast method with different volume fractions of PANI varying from 0.04% to 0.048% of PANI content. The films are characterized for structural, mechanical, and surface morphological properties using X-ray diffraction, differential scanning calorimeter, Raman spectra, Infrared spectra, tensile testing, and scanning electron microscopy. The X-ray diffraction analysis shows that, prepared films were in β-phase. The DSC scans indicated that the degree of crystallinity in PVDF-PANI is improved. Raman and Infrared spectrum further confirm the presence of β-phase of PVDF-PANI film. Tensile properties of PVDF-PANI films were in good agreement with those reported in literature. The surface feature shows that PANI is uniformly distributed in PVDF and also results in disappearance of spherulites. The influence of volume fraction of PANI in PVDF on dielectric properties was analyzed. The results showed that the dielectric permittivity of PVDF-PANI (120) was much higher than that of PVDF (12). The sensitivity of these films was studied on application of a pressure and a constant output voltage was obtained.

Keywords: dielectric Properties, PANI, PVDF, smart materials

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Authors: Branko Skoric, Aleksandar Miletic, Pal Terek, Lazar Kovacevic, Milan Kukuruzovic

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In this paper, we present the results of a study of TiN thin films which are deposited by a Physical Vapour Deposition (PVD) and Ion Beam Assisted Deposition (IBAD). In the present investigation the subsequent ion implantation was provided with N⁵⁺ ions. The ion implantation was applied to enhance the mechanical properties of surface. The thin film deposition process exerts a number of effects such as crystallographic orientation, morphology, topography, densification of the films. A variety of analytic techniques were used for characterization, such as scratch test, calo test, Scanning electron microscopy (SEM), Atomic Force Microscope (AFM), X-ray diffraction (XRD) and Energy Dispersive X-ray analysis (EDAX).

Keywords: coating, super hard, ion implantation, nanohardness

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Authors: H. K. G. K. D. K. Hapuhinna, R. D. Gunaratne, H. M. J. C. Pitawala

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Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.

Keywords: dentistry, Eppawala chlorapatite, hydroxyapatite, orthopedics

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Authors: Soma Ghosh, Balaram Mohapatra, Pinaki Sar, Abhijeet Mukherjee

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Microbial role in arsenic (As) mobilization in the groundwater aquifers of Brahmaputra river basin (BRB) in India, severely threatened by high concentrations of As, remains largely unknown. The present study, therefore, is a molecular and ecophysiological characterization of an indigenous bacterium strain IIIJ3-1 isolated from As contaminated groundwater of BRB and application of this strain in several microcosm set ups differing in their organic carbon (OC) source and terminal electron acceptors (TEA), to understand its role in As dissolution under aerobic and anaerobic conditions. Strain IIIJ3-1 was found to be a new facultative anaerobic, gram-positive, endospore-forming strain capable of arsenite (As3+) oxidation and dissimilatory arsenate (As5+) reduction. The bacterium exhibited low genomic (G+C)% content (45 mol%). Although, its 16S rRNA gene sequence revealed a maximum similarity of 99% with Bacillus cereus ATCC 14579(T) but the DNA-DNA relatedness of their genomic DNAs was only 49.9%, which remains well below the value recommended to delimit different species. Abundance of fatty acids iC17:0, iC15:0 and menaquinone (MK) 7 though corroborates its taxonomic affiliation with B. cereus sensu-lato group, presence of hydroxy fatty acids (HFAs), C18:2, MK5 and MK6 marked its uniqueness. Besides being highly As resistant (MTC=10mM As3+, 350mM As5+), metabolically diverse, efficient aerobic As3+ oxidizer; it exhibited near complete dissimilatory reduction of As5+ (1 mM). Utilization of various carbon sources with As5+ as TEA revealed lactate to serve as the best electron donor. Aerobic biotransformation assay yielded a lower Km for As3+ oxidation than As5+ reduction. Arsenic homeostasis was found to be conferred by the presence of arr, arsB, aioB, and acr3(1) genes. Scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) analysis of this bacterium revealed reduction in cell size upon exposure to As and formation of As-rich electron opaque dots following growth with As3+. Incubation of this strain with sediment (sterilised) collected from BRB aquifers under varying OC, TEA and redox conditions revealed that the strain caused highest As mobilization from solid to aqueous phase under anaerobic condition with lactate and nitrate as electron donor and acceptor, respectively. Co-release of highest concentrations of oxalic acid, a well known bioweathering agent, considerable fold increase in viable cell counts and SEM-EDX and X-ray diffraction analysis of the sediment after incubation under this condition indicated that As release is consequent to microbial bioweathering of the minerals. Co-release of other elements statistically proves decoupled release of As with Fe and Zn. Principle component analysis also revealed prominent role of nitrate under aerobic and/or anaerobic condition in As release by strain IIIJ3-1. This study, therefore, is the first to isolate, characterize and reveal As mobilization property of a strain belonging to the Bacillus cereus sensu lato group isolated from highly As contaminated aquifers of Brahmaputra River Basin.

Keywords: anaerobic microcosm, arsenic rich electron opaque dots, Arsenic release, Bacillus strain IIIJ3-1

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Authors: Aboozar Aghaei

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In the present work, the dissimilar Monel400 and SS316 were joined by friction stir welding (FSW). The applied rotating speed was 400 rpm, whereas the traverse speed varied between 50 and 150 mm/min. At a constant rotating speed, the sound welds were obtained at the welding speeds of 50 and 100 mm/min. However, a groove-like defect was formed when the welding speed exceeded 100 mm/min. The mechanical properties of the joints were evaluated using tensile and fatigue tests. The fatigue strength of dissimilar FSWed specimen was higher than that of both Monel400 and SS316. To study the failure behavior of FSWed specimens, the fracture surfaces were analyzed using scanning electron microscope (SEM). The failure analysis indicates that different mechanisms may contribute to the fracture of welds. This was attributed to the dissimilar characteristics of dissimilar materials exhibiting different failure behaviors.

Keywords: mechanical properties, stainless steel, frictions, monel

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Authors: D. Korsacilar, C. Atas

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In this study, first thermoplastic composite materials/plates that have high ballistic impact resistance were produced. For this purpose, the thermoplastic prepreg and the vacuum bagging technique were used to produce a composite material. Thermoplastic prepregs (resin-impregnated fiber) that are supplied ready to be used, namely high-density polyethylene (HDPE) was chosen as matrix and unidirectional glass fiber was used as reinforcement. In order to compare the fiber configuration effect on mechanical properties, unidirectional and biaxial prepregs were used. Then the microstructural properties of the composites were investigated with scanning electron microscopy (SEM) analysis. Impact properties of the composites were examined by Charpy impact test and tensile mechanical tests and then the effects of ultraviolet irradiation were investigated on mechanical performance.

Keywords: ballistic, composite, thermoplastic, prepreg

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

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Ternary nanocomposites based on hydroxyapatite (HAP) and alumina (Al2O3) were embedded through graphene oxide (GO) nanosheets to be investigated for medical applications. The composition of the preparations has been confirmed by X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and Fourier-Transform infrared spectroscopy. Scanning and transmission electron microscopy have shown the typical morphologies of the components of the nanocomposites with hydroxyapatite nanorods reaching an average diameter of 22.26±2 nm and an average length of 69.56±19.25 nm in the ternary nanocomposites. The ternary nanocomposite has a microhardness of 5.8±0.1 GPa and a higher average roughness of 6.5 nm compared to pure HAP preparation with an average roughness of 2.7 nm. All preparations have shown an acceptable cytotoxicity profile with a percent osteoblasts cell viability of 98.6±1.3% after culturing with the ternary nanocomposite. The TNC has also shown the highest antibacterial activity compared to preparations of each of its constituents and their nanocomposites, with a zone of inhibition’s diameter of 14.1±0.8 mm and 13.6±0.6 mm against Staphylococcus aureus and Escherichia coli, respectively, compared to no zone of inhibition for the pure hydroxyapatite preparation.

Keywords: hydroxypatite, cytotoxicity, nanocomposites, X-ray analysis

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Authors: Rajkumar Ghosh

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The paper presents a comprehensive study of the structural analysis of the Chaura Thrust in Himachal Pradesh, India. The research focuses on several key aspects, including the activation timing of the Main Central Thrust (MCT) and the South Tibetan Detachment System (STDS), the identification and characterization of mylonitised zones through microscopic examination, and the understanding of box fold characteristics and their implications in the regional geology of the Himachal Himalaya. The primary objective of the study is to provide field documentation of the Chaura Thrust, which was previously considered a blind thrust with limited field evidence. Additionally, the research aims to characterize box folds and their signatures within the broader geological context of the Himachal Himalaya, document the temperature range associated with grain boundary migration (GBM), and explore the overprinting structures related to multiple sets of Higher Himalayan Out-of-Sequence Thrusts (OOSTs). The research methodology employed geological field observations and microscopic studies. Samples were collected along the Jhakri-Chaura transect at regular intervals of approximately 1 km to conduct strain analysis. Microstructural studies at the grain scale along the Jhakri-Wangtu transect were used to document the GBM-associated temperature range. The study reveals that the MCT activated in two parts, as did the STDS, and provides insights into the activation ages of the Main Boundary Thrust (MBT) and the Main Frontal Thrust (MFT). Under microscopic examination, the study identifies two mylonitised zones characterized by S-C fabric, and it documents dynamic and bulging recrystallization, as well as sub-grain formation. Various types of crenulated schistosity are observed in photomicrographs, including a rare occurrence where crenulation cleavage and sigmoid Muscovite are found juxtaposed. The study also notes the presence of S/SE-verging meso- and micro-scale box folds around Chaura, which may indicate structural upliftment. Kink folds near Chaura are visible, while asymmetric shear sense indicators in augen mylonite are predominantly observed under microscopic examination. Moreover, the research highlights the documentation of the Higher Himalayan Out-of-Sequence Thrust (OOST) in Himachal Pradesh, which activated the MCT and occurred within a zone south of the Main Central Thrust Upper (MCTU). The presence of multiple sets of OOSTs suggests a zigzag pattern of strain accumulation in the area. The study emphasizes the significance of understanding the overprinting structures associated with OOSTs. Overall, this study contributes to the understanding of the structural analysis of the Chaura Thrust and its implications in the regional geology of the Himachal Himalaya. The research underscores the importance of microscopic studies in identifying mylonitised zones and various types of crenulated schistosity. Additionally, the study documents the GBM-associated temperature range and provides insights into the activation of the Higher Himalayan Out-of-Sequence Thrust (OOST) in Himachal Pradesh. The findings of the study were obtained through geological field observations, microscopic studies, and strain analysis, offering valuable insights into the activation timing, mylonitization characteristics, and overprinting structures related to the Chaura Thrust and the broader tectonic framework of the region.

Keywords: Main Central Thrust, Jhakri Thrust, Chaura Thrust, Higher Himalaya, Out-of-Sequence Thrust, Sarahan Thrust

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Authors: H. Maachou, A. Chagnes, G. Cote

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The present work reports the properties of chitosan/hydroxyapatite (Cs/HA: 100/00, 70/30 and 30/70) composite microspheres obtained by emulsification processing route. The morphology of chitosane microspheres was observed by a scanning electron microscope (SEM) which shows an aggregate of spherical microspheres with a particle size, determined by optical microscope, ranged from 4 to 10 µm. Thereafter, a biomimetic approach was used to study the in vitro biomineralization of these composites. It concerns the composites immersion in simulated body fluid (SBF) for different times. The deposited calcium phosphate was studied using X-ray diffraction analysis (XRD), FTIR spectroscopy and ICP analysis of phosphorus. In fact, the mineral formed on Cs/HA microspheres was a mixture of carbonated HA and β-TCP as showed by FTIR peaks at 1419,5 and 871,8 cm-1 and XRD peak at 29,5°. This formation was induced by the presence of HA in chitosan microspheres. These results are confirmed by SEM micrographs which chow the Ca-P crystals growth in form of cauliflowers. So, these materials are of great interest for bone regeneration applications due to their ability to nucleate calcium phosphates in presence of simulated body fluid (SBF).

Keywords: hydroxyapatite, chitosan, microsphere, composite, bone regeneration

Procedia PDF Downloads 309