Search results for: broadband dielectric spectroscopy

Authors: Mourad Makhlouf, Bouabdellah Benaicha, Zoubir Benmaamar, Didier Villemin

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The addition of combustion catalysts to ammonium perchlorate-based composite fuels can indeed significantly enhance their performance. In this work, a nanocomposite was synthesized using graphene oxide (GO) and hematite nanoparticles grafted onto graphene oxide as a catalyst support.To characterize the nanocomposite, several experimental techniques were employed, including Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM). FTIR is useful for analyzing chemical bonding and functional groups, while Raman spectroscopy provides information about the vibrational modes of the materials. SEM allows for visualizing the surface morphology and structure.The thermal analysis of two mixtures, one based on AP/GO and the other on AP/GO-Fe2O3, was conducted with varying percentages. The results indicated that the nanocomposite GO-Fe2O3 acted as a catalyst, significantly accelerating the thermal decomposition process of AP. This catalytic effect ultimately led to an improvement in the energy performance of the composite fuel.Overall, the synthesis and characterization of the nanocomposite, as well as the thermal analysis, demonstrated the effectiveness of GO-Fe2O3 as a combustion catalyst in enhancing the performance of ammonium perchlorate-based composite fuels.

Keywords: composite propellants, ammonium perchlorate, nanocomposite, catalytic support, hematite nanoparticles, graphene oxide, thermal decomposition

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Authors: Asiful Hossain Seikh, Mohammad Asif Alam, Ubair Abdus Samad, Jabair A. Mohammed, S. M. Al-Zahrani, El-Sayed M. Sherif

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In this current investigation, aliphatic amine-cured diglycidyl ether of bisphenol-A (DGEBA) based epoxy coating was mixed with certain weight % hardener polyaminoamide (1:2) and was coated on carbon steel panels with and without 1% nano crystalline Al powder. The corrosion behavior of the coated samples were investigated by exposing them in the salt spray chamber, for 500 hours. According to ASTM-B-117, the bath was kept at 35 °C and 5% NaCl containing mist was sprayed at 1.3 bars pressure. Composition of coatings was confirmed using Fourier-transform infrared spectroscopy (FTIR). Electrochemical characterization of the coated samples was also performed using potentiodynamic polarization technique and electrochemical impedance spectroscopy (EIS) technique. All the experiments were done in 3.5% NaCl solution. The nano Al coated sample shows good corrosion resistance property compared to bare Al sample. In fact after salt spray exposure no pitting or local damage was observed for nano coated sample and the coating gloss was negligibly affected. The surface morphology of coated and corroded samples was studied using scanning electron microscopy (SEM).

Keywords: epoxy, nano aluminium, potentiodynamic polarization, salt spray, electrochemical impedence spectroscopy

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Authors: Dana Alina Magdas, Nicoleta Simona Vedeanu, Ioana Feher, Rares Stiufiuc

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Food and beverages authentication using rapid and non-expensive analytical tools represents nowadays an important challenge. In this regard, the potential of vibrational techniques in food authentication has gained an increased attention during the last years. For wines discrimination, Raman spectroscopy appears more feasible to be used as compared with IR (infrared) spectroscopy, because of the relatively weak water bending mode in the vibrational spectroscopy fingerprint range. Despite this, the use of Raman technique in wine discrimination is in an early stage. Taking this into consideration, the wine discrimination potential of surface-enhanced Raman scattering (SERS) technique is reported in the present work. The novelty of this study, compared with the previously reported studies, concerning the application of vibrational techniques in wine discrimination consists in the fact that the present work presents the wines differentiation based on the individual signals obtained from deconvoluted spectra. In order to achieve wines classification with respect to variety, geographical origin and vintage, the peaks intensities obtained after spectra deconvolution were compared using supervised chemometric methods like Linear Discriminant Analysis (LDA). For this purpose, a set of 20 white Romanian wines from different viticultural Romanian regions four varieties, was considered. Chemometric methods applied directly to row SERS experimental spectra proved their efficiency, but discrimination markers identification found to be very difficult due to the overlapped signals as well as for the band shifts. By using this approach, a better general view related to the differences that appear among the wines in terms of compositional differentiation could be reached.

Keywords: chemometry, SERS, variety, wines discrimination

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Authors: Akhtar Rasool, Tasneem Zahra Rizvi

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In this study, a series of the cadmium sulphide quantum dots/polyaniline nanocomposites with varying compositions were prepared by in-situ polymerization technique and were characterized using X-ray diffraction and Fourier transform infrared spectroscopy. The surface morphology was studied by scanning electron microscopy. UV-Visible spectroscopy was used to find out the energy band gap of the nanoparticles and the nanocomposites. Temperature dependence of DC electrical conductivity and temperature and frequency dependence of AC conductivity were investigated to study the charge transport mechanism in the nanocomposites. DC conductivity was found to be a typical for a semiconducting behavior following Mott’s 1D variable range hoping model. The frequency dependent AC conductivity followed the universal power law.

Keywords: conducting polymers, nanocomposites, polyaniline composites, quantum dots

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Authors: Amanda T. Badaró, Douglas F. Barbin, Sofia T. Garcia, Maria Teresa P. S. Clerici, Amanda R. Ferreira

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Food fortification is the intentional addition of a nutrient in a food matrix and has been widely used to overcome the lack of nutrients in the diet or increasing the nutritional value of food. Fortified food must meet the demand of the population, taking into account their habits and risks that these foods may cause. Wheat and its by-products, such as semolina, has been strongly indicated to be used as a food vehicle since it is widely consumed and used in the production of other foods. These products have been strategically used to add some nutrients, such as fibers. Methods of analysis and quantification of these kinds of components are destructive and require lengthy sample preparation and analysis. Therefore, the industry has searched for faster and less invasive methods, such as Near-Infrared Spectroscopy (NIR). NIR is a rapid and cost-effective method, however, it is based on indirect measurements, yielding high amount of data. Therefore, NIR spectroscopy requires calibration with mathematical and statistical tools (Chemometrics) to extract analytical information from the corresponding spectra, as Principal Component Analysis (PCA) and Linear Discriminant Analysis (LDA). PCA is well suited for NIR, once it can handle many spectra at a time and be used for non-supervised classification. Advantages of the PCA, which is also a data reduction technique, is that it reduces the data spectra to a smaller number of latent variables for further interpretation. On the other hand, LDA is a supervised method that searches the Canonical Variables (CV) with the maximum separation among different categories. In LDA, the first CV is the direction of maximum ratio between inter and intra-class variances. The present work used a portable infrared spectrometer (NIR) for identification and classification of pure and fiber-fortified semolina samples. The fiber was added to semolina in two different concentrations, and after the spectra acquisition, the data was used for PCA and LDA to identify and discriminate the samples. The results showed that NIR spectroscopy associate to PCA was very effective in identifying pure and fiber-fortified semolina. Additionally, the classification range of the samples using LDA was between 78.3% and 95% for calibration and 75% and 95% for cross-validation. Thus, after the multivariate analysis such as PCA and LDA, it was possible to verify that NIR associated to chemometric methods is able to identify and classify the different samples in a fast and non-destructive way.

Keywords: Chemometrics, fiber, linear discriminant analysis, near-infrared spectroscopy, principal component analysis, semolina

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Authors: Marta Chiapasco, Alexandra Porter, Finn Giuliani

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Designing polymers with a specific microstructure can affect how the polymer degrades once released in the environment. Not only the amount but also the distribution of different phases determines a polymers’ degradability. The following research investigates the use of a combination of spectroscopy analysis and thermal analysis to study changes of polymers’ amorphous and crystalline phases during degradation, comparing different microstructures of polypropylene and polyethylene. The use of nanoindentation helps study how degradation proceeds across a material by looking at changes in phases, while bulk tensile test describes when the material fails. The first results demonstrate that different microstructures have different degrading rates, with homopolymer having a linear and faster degradation compared to copolymers. The goal is to create materials that degrade at faster rates without releasing microplastics into the environment.

Keywords: degradation, microstructure, nanoindentation, Raman spectroscopy

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Authors: Ahmed A. Al-Amiery, Yasmin K. Al-Majedy, Abdul Amir H. Kadhum, Abu Bakar Mohamad

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The efficiency of synthesized thiosemicarbazone namely 2-(1,5-dimethyl-4-(2-methylbenzylidene)amino)-2-phenyl-1H-pyrazol-3(2H)-ylidene) hydrazinecarbothioamide investigated as corrosion inhibitor of mild steel in 1N H2SO4 using electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization (PD) in addition of scanning electron microscopy (SEM). The results showed that this inhibitor behaved as a good corrosion inhibitor even at low concentration with a mean efficiency of 93%. Polarization technique and EIS were tested in different concentrations reveal that this compound is adsorbed on the mild steel, therefore blocking the active sites and the adsorption follows the Langmuir adsorption isotherm model. SEM shows that mild steel surface is nearly perfect for mild steel which was immersed in a solution of H2SO4 with corrosion inhibitor.

Keywords: corrosion inhibitor, thiosemicarbazide, electrochemical impedance, electrochemical impedance spectroscopy

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Authors: Valeriy M. Kondratev, Ekaterina A. Vyacheslavova, Talgat Shugabaev, Alexander S. Gudovskikh, Alexey D. Bolshakov

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Modern sensorics imposes strict requirements on the biosensors characteristics, especially technological feasibility, and selectivity. There is a growing interest in the analysis of human health biological markers, which indirectly testifying the pathological processes in the body. Such markers are acids and alkalis produced by the human, in particular - ammonia and hydrochloric acid, which are found in human sweat, blood, and urine, as well as in gastric juice. Biosensors based on modern nanomaterials, especially low dimensional, can be used for this markers detection. Most classical adsorption sensors based on metal and silicon oxides are considered non-selective, because they identically change their electrical resistance (or impedance) under the action of adsorption of different target analytes. This work demonstrates a feasible frequency-resistive method of electrical impedance spectroscopy data analysis. The approach allows to obtain of selectivity in adsorption sensors of a resistive type. The method potential is demonstrated with analyzis of impedance spectra of silicon nanowires in the presence of NH3 and HCl vapors with concentrations of about 125 mmol/L (2 ppm) and water vapor. We demonstrate the possibility of unambiguous distinction of the sensory signal from NH3 and HCl adsorption. Moreover, the method is found applicable for analysis of the composition of ammonia and hydrochloric acid vapors mixture without water cross-sensitivity. Presented silicon sensor can be used to find diseases of the gastrointestinal tract by the qualitative and quantitative detection of ammonia and hydrochloric acid content in biological samples. The method of data analysis can be directly translated to other nanomaterials to analyze their applicability in the field of biosensory.

Keywords: electrical impedance spectroscopy, spectroscopy data analysis, selective adsorption sensor, nanotechnology

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Authors: Chen-Fu Wang, Lin-Ya Kung

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For traditional painting materials, the artisan used to combine the pigments with different binders to create colors. As time goes by, the materials used for painting evolved from natural to chemical materials. The vast variety of ingredients used in chemical materials has complicated restoration work; it makes conservation work more difficult. Conservation work also becomes harder when the materials cannot be easily identified; therefore, it is essential that we take a more scientific approach to assist in conservation work. Paintings materials are high molecular weight polymer, and their analysis is very complicated as well other contamination such as smoke and dirt can also interfere with the analysis of the material. The current methods of composition analysis of painting materials include Fourier transform infrared spectroscopy (FT-IR), mass spectrometer, Raman spectroscopy, X-ray diffraction spectroscopy (XRD), each of which has its own limitation. In this study, FT-IR was used to analyze the components of the paint coating. We have taken the most commonly seen materials as samples and deteriorated it. The aged information was then used for the database to exam the temple painting materials. By observing the FT-IR changes over time, we can tell all of the painting materials will be deteriorated by the UV light, but only the speed of its degradation had some difference. From the deterioration experiment, the acrylic resin resists better than the others. After collecting the painting materials aging information on FT-IR, we performed some test on the paintings on the temples. It was found that most of the artisan used tune-oil for painting materials, and some other paintings used chemical materials. This method is now working successfully on identifying the painting materials. However, the method is destructive and high cost. In the future, we will work on the how to know the painting materials more efficiently.

Keywords: temple painting, painting material, conservation, FT-IR

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Authors: Ashiq Hussain, Mahwash Hussain, Zeenat Parveen

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Now a days the demand for broadband service has increased. Due to which the researchers are trying to find a solution to provide a large amount of service. There is a shortage of bandwidth because of the use of downloading video, voice and data. One of the solutions to overcome this shortage of bandwidth is to provide the communication system with passive optical components. We have increased the data rate in this system. From experimental results we have concluded that the quality factor has increased by adding passive optical networks.

Keywords: WDM-PON, optical fiber, BER, Q-factor, eye diagram

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Authors: Duygu Çimen, Nilay Bereli, Adil Denizli

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In this study is to synthesis magnetic nanoparticles for purify protein C. For this aim, N-Methacryloyl-(L)-histidine methyl ester (MAH) containing 2-hydroxyethyl methacrylate (HEMA) based magnetic nanoparticles were synthesized by using micro-emulsion polymerization technique for templating protein C via metal chelation. The obtained nanoparticles were characterized with Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), zeta-size analysis and electron spin resonance (ESR) spectroscopy. After that, they were used for protein C purification from aqueous solution to evaluate/optimize the adsorption condition. Hereby, the effecting factors such as concentration, pH, ionic strength, temperature, and reusability were evaluated. As the last step, protein C was determined with sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

Keywords: immobilized metal affinity chromatography (IMAC), magnetic nanoparticle, protein C, hydroxyethyl methacrylate (HEMA)

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Authors: Anna S. Tolkacheva, Sergey N. Shkerin, Kirill G. Zemlyanoi, Olga G. Reznitskikh, Pavel D. Khavlyuk

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Calcium oxovanadates with garnet related structure are multifunctional oxides in various fields like photoluminescence, microwave dielectrics, and magneto-dielectrics. For example, vanadate garnets are self-luminescent compounds. They attract attention as RE-free broadband excitation and emission phosphors and are candidate materials for UV-based white light-emitting diodes (WLEDs). Ca₅M₄(VO₄)₆ (M = Mg, Zn, Co, Ni, Mn) compounds are also considered promising for application in microwave devices as substrate materials. However, the relation between their structure, composition and physical/chemical properties remains unclear. Given the above-listed observations, goals of this study are to synthesise Ca₅M₄(VO₄)₆ (M = Mg, Zn, Ni) and to study their thermal and electrical properties. Solid solutions Ca₅Mg₄₋ₓMₓ(VO₄)₆ (0 ≤ x ≤ 4) where M is Zn and Ni have been synthesized by sol-gel method. The single-phase character of the final products was checked by powder X-ray diffraction on a Rigaku D/MAX-2200 X-ray diffractometer using Cu Kα radiation in the 2θ range from 15° to 70°. The dependence of thermal properties on chemical composition of solid solutions was studied using simultaneous thermal analyses (DSC and TG). Thermal analyses were conducted in a Netzch simultaneous analyser STA 449C Jupiter, in Ar atmosphere, in temperature range from 25 to 1100°C heat rate was 10 K·min⁻¹. Coefficients of thermal expansion (CTE) were obtained by dilatometry measurements in air up to 800°C using a Netzsch 402PC dilatometer; heat rate was 1 K·min⁻¹. Impedance spectra were obtained via the two-probe technique with an impedance meter Parstat 2273 in air up to 700°C with the variation of pH₂O from 0.04 to 3.35 kPa. Cation deficiency in Ca and Mg sublattice under the substitution of MgO with ZnO up to 1/6 was observed using Rietveld refinement of the crystal structure. Melting point was found to decrease with x changing from 0 to 4 in Ca₅Mg₄₋ₓMₓ(VO₄)₆ where M is Zn and Ni. It was observed that electrical conductivity does not depend on air humidity. The reported study was funded by the RFBR Grant No. 17–03–01280. Sample attestation was carried out in the Shared Access Centers at the IHTE UB RAS.

Keywords: garnet structure, electrical conductivity, thermal expansion, thermal properties

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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: Manish Saha, Manish Kumar Niranjan, Saket Asthana

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The K₀.₅Na₀.₅NbO₃ (KNN) system has emerged as one of the most promising lead-free piezoelectric over the years. In this work, we perform a comprehensive investigation of electronic structure, lattice dynamics and dielectric/ferroelectric properties of the room temperature phase of KNN by combining ab-initio DFT-based theoretical analysis and experimental characterization. We assign the symmetry labels to KNN vibrational modes and obtain ab-initio polarized Raman spectra, Infrared (IR) reflectivity, Born-effective charge tensors, oscillator strengths etc. The computed Raman spectrum is found to agree well with the experimental spectrum. In particular, the results suggest that the mode in the range ~840-870 cm-¹ reported in the experimental studies is longitudinal optical (LO) with A_1 symmetry. The Raman mode intensities are calculated for different light polarization set-ups, which suggests the observation of different symmetry modes in different polarization set-ups. The electronic structure of KNN is investigated, and an optical absorption spectrum is obtained. Further, the performances of DFT semi-local, metal-GGA and hybrid exchange-correlations (XC) functionals, in the estimation of KNN band gaps are investigated. The KNN bandgap computed using GGA-1/2 and HSE06 hybrid functional schemes are found to be in excellant agreement with the experimental value. The COHP, electron localization function and Bader charge analysis is also performed to deduce the nature of chemical bonding in the KNN. The solid-state reaction and hydrothermal methods are used to prepare the KNN ceramics, and the effects of grain size on the physical characteristics these ceramics are examined. A comprehensive study on the impact of different synthesis techniques on the structural, electrical, and photocatalytic properties of ferroelectric ceramics KNN. The KNN-S prepared by solid-state method have significantly larger grain size as compared to that for KNN-H prepared by hydrothermal method. Furthermore, the KNN-S is found to exhibit higher dielectric, piezoelectric and ferroelectric properties as compared to KNN-H. On the other hand, the increased photocatalytic activity is observed in KNN-H as compared to KNN-S. As compared to the hydrothermal synthesis, the solid-state synthesis causes an increase in the relative dielectric permittivity (ε^') from 2394 to 3286, remnant polarization (P_r) from 15.38 to 20.41 μC/cm^², planer electromechanical coupling factor (k_p) from 0.19 to 0.28 and piezoelectric coefficient (d_33) from 88 to 125 pC/N. The KNN-S ceramics are also found to have a lower leakage current density, and higher grain resistance than KNN-H ceramic. The enhanced photocatalytic activity of KNN-H is attributed to relatively smaller particle sizes. The KNN-S and KNN-H samples are found to have degradation efficiencies of RhB solution of 20% and 65%, respectively. The experimental study highlights the importance of synthesis methods and how these can be exploited to tailor the dielectric, piezoelectric and photocatalytic properties of KNN. Overall, our study provides several bench-mark important results on KNN that have not been reported so far.

Keywords: lead-free piezoelectric, Raman intensity spectrum, electronic structure, first-principles calculations, solid state synthesis, photocatalysis, hydrothermal synthesis

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Authors: Natsumi Murakami, Jae-Ho Kim, Susumu Yonezawa

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The calcium fluorosilicate (CaSiF₆) was prepared from calcium silicate (CaSiO₃) with fluorine gas at 25 ~ 200 ℃ and 760 Torr for 1~24 h. Especially, the pure CaSiF₆ could be prepared at 25 ℃ for 24 h with F₂ gas from the results of X-ray diffraction. Increasing temperature to higher than 100 ℃, the prepared CaSiF₆ was decomposed into CaF₂ and SiF₄. The release of SiF₄ gas was confirmed by the results of gas-phase infrared spectroscopy. In this study, we tried to modify the surface of polycarbonate (PC) resin using the SiF₄ gas released from CaSiF₆ particles. By using the prepared CaSiF₆, the surface roughness of fluorinated PC samples was approximately four times larger than that (1.4 nm) of the untreated sample. The results of X-ray photoelectron spectroscopy indicated the formation of fluorinated bonds (e.g., -CFx) on the surface of PC after surface fluorination. Consequently, the CaSiF₆ particles can be useful for a new fluorinating agent.

Keywords: calcium fluorosilicate, fluorinating agent, polycarbonate, surface fluorination

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Authors: M. Kalbac, T. Verhagen, K. Drogowska, J. Vejpravova

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One- and two-dimensional carbon nano structures with sp2 hybridization of carbon atoms (single walled carbon nano tubes and graphene) are promising materials in future electronic and spintronics devices due to specific character of their electronic structure. In this paper, we present a comparative study of graphene and single-wall carbon nano tubes by Raman spectro-microscopy in strong magnetic field. This unique method allows to study changes in electronic band structure of the two types of carbon nano structures induced by a strong magnetic field.

Keywords: carbon nano structures, magnetic field, raman spectroscopy, spectro-microscopy

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Authors: R. Buntem, K. Samkongngam

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The silicate glass was prepared using rice husk as the source of silica. The base composition of glass sample is composed of SiO2 (from rice husk ash), Na2CO3, K2CO3, ZnO, H3BO3, CaO, Al2O3 or Al, and CuO. Aluminum is used in place of Al2O3 in order to reduce Cu2+ to Cu+. The red color of Cu2O in the glass matrix was observed when the Al was added into the glass mixture. The expansion coefficients of the copper doped glass are in the range of 1.2 x 10-5-1.4x10-5 (ºC -1) which is common for the silicate glass. The finger prints of the bond vibrations were studied using IR spectroscopy. While the oxidation state and the coordination information of the copper ion in the glass matrix were investigated using X-ray absorption spectroscopy. From the data, Cu+ and Cu2+ exist in the glass matrix. The red particles of Cu2O can be formed in the glass matrix when enough aluminum was added.

Keywords: copper in glass, coordination information, silicate glass, XANES spectrum

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Authors: Irmak Gunes Yuceil

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This paper outlines interferences and analytical errors which are encountered in the qualification and quantification of archaeological and ethnographic artifacts, by means of handheld x-ray fluorescence. These shortcomings were evaluated through case studies carried out on metallic artifacts related to various periods and cultures around Anatolia. An Innov-X Delta Standard 2000 handheld x-ray fluorescence spectrometer was used to collect data from 1361 artifacts, through 6789 measurements and 70 hours’ tube usage, in between 2013-2017. Spectrum processing was done by Delta Advanced PC Software. Qualitative and quantitative results screened by the device were compared with the spectrum graphs, and major discrepancies associated with physical and analytical interferences were clarified in this paper.

Keywords: hand-held x-ray fluorescence spectroscopy, art and archaeology, interferences and analytical errors, pre-diagnosis in conservation

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Authors: Rajnish Shrivastava, Y. R. Sood, Priti Pundir, Rahul Srivastava

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Power transformer is one of the most important devices that are used in power station. Due to several fault impending upon it or due to ageing, etc its life gets lowered. So, it becomes necessary to have diagnosis of oil for fault analysis. Due to the chemical, electrical, thermal and mechanical stress the insulating material in the power transformer degraded. It is important to regularly assess the condition of oil and the remaining life of the power transformer. In this paper UV-VIS absorption graph area is correlated with moisture content, Flash point, IFT and Density of Transformer oil. Since UV-VIS absorption graph area varies accordingly with the variation in different transformer parameters. So by obtaining the correlation among different oil parameters for oil with respect to UV-VIS absorption area, decay contents of transformer oil can be predicted

Keywords: breakdown voltage (BDV), interfacial Tension (IFT), moisture content, ultra violet-visible rays spectroscopy (UV-VIS)

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Authors: Sultan Ben Jaber

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Optical properties of molecules exhibit dramatic changes when adsorbed close to nano-structure metallic surfaces such as gold and silver nanomaterial. This phenomena opened a wide range of research to improve conventional spectroscopies efficiency. A well-known technique that has an intensive focus of study is surface-enhanced Raman spectroscopy (SERS), as since the first observation of SERS phenomena, researchers have published a great number of articles about the potential mechanisms behind this effect as well as developing materials to maximize the enhancement. Infrared and Raman spectroscopy are complementary techniques; thus, surface-enhanced infrared absorption (SEIRA) also shows a noticeable enhancement of molecules in the mid-IR excitation on nonmetallic structure substrates. In the SEIRA, vibrational modes that gave change in dipole moments perpendicular to the nano-metallic substrate enhanced 200 times greater than the free molecule’s modes. SEIRA spectroscopy is promising for the characterization and identification of adsorbed molecules on metallic surfaces, especially at trace levels. IR reflection-absorption spectroscopy (IRAS) is a well-known technique for measuring IR spectra of adsorbed molecules on metallic surfaces. However, SEIRA spectroscopy sensitivity is up to 50 times higher than IRAS. SEIRA enhancement has been observed for a wide range of molecules adsorbed on metallic substrates such as Au, Ag, Pd, Pt, Al, and Ni, but Au and Ag substrates exhibited the highest enhancement among the other mentioned substrates. In this work, trace levels of 3,4-methylenedioxymethamphetamine (MDMA) have been detected using gold nanoparticles (AuNPs) substrates with surface-enhanced infrared absorption (SEIRA). AuNPs were first prepared and washed, then mixed with different concentrations of MDMA samples. The process of fabricating the substrate prior SEIRA measurements included mixing of AuNPs and MDMA samples followed by vigorous stirring. The stirring step is particularly crucial, as stirring allows molecules to be robustly adsorbed on AuNPs. Thus, remarkable SEIRA was observed for MDMA samples even at trace levels, showing the rigidity of our approach to preparing SEIRA substrates.

Keywords: surface-enhanced infrared absorption (SEIRA), gold nanoparticles (AuNPs), amphetamines, methylene dioxy- methamphetamine (MDMA), enhancement factor

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Authors: Elena B. Cherepetskaya, Alexander A. Karabutov, Natalia B. Podymova, Ivan Sas

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Nonlinear evolution of broadband ultrasonic pulses passed through the rock specimens is studied using the apparatus ‘GEOSCAN-02M’. Ultrasonic pulses are excited by the pulses of Q-switched Nd:YAG laser with the time duration of 10 ns and with the energy of 260 mJ. This energy can be reduced to 20 mJ by some light filters. The laser beam radius did not exceed 5 mm. As a result of the absorption of the laser pulse in the special material – the optoacoustic generator–the pulses of longitudinal ultrasonic waves are excited with the time duration of 100 ns and with the maximum pressure amplitude of 10 MPa. The immersion technique is used to measure the parameters of these ultrasonic pulses passed through a specimen, the immersion liquid is distilled water. The reference pulse passed through the cell with water has the compression and the rarefaction phases. The amplitude of the rarefaction phase is five times lower than that of the compression phase. The spectral range of the reference pulse reaches 10 MHz. The cubic-shaped specimens of the Karelian gabbro are studied with the rib length 3 cm. The ultimate strength of the specimens by the uniaxial compression is (300±10) MPa. As the reference pulse passes through the area of the specimen without cracks the compression phase decreases and the rarefaction one increases due to diffraction and scattering of ultrasound, so the ratio of these phases becomes 2.3:1. After preloading some horizontal cracks appear in the specimens. Their location is found by one-sided scanning of the specimen using the backward mode detection of the ultrasonic pulses reflected from the structure defects. Using the computer processing of these signals the images are obtained of the cross-sections of the specimens with cracks. By the increase of the reference pulse amplitude from 0.1 MPa to 5 MPa the nonlinear transformation of the ultrasonic pulse passed through the specimen with horizontal cracks results in the decrease by 2.5 times of the amplitude of the rarefaction phase and in the increase of its duration by 2.1 times. By the increase of the reference pulse amplitude from 5 MPa to 10 MPa the time splitting of the phases is observed for the bipolar pulse passed through the specimen. The compression and rarefaction phases propagate with different velocities. These features of the powerful broadband ultrasonic pulses passed through the rock specimens can be described by the hysteresis model of Preisach-Mayergoyz and can be used for the location of cracks in the optically opaque materials.

Keywords: cracks, geological materials, nonlinear evolution of ultrasonic pulses, rock

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Authors: Nader Nciri, Suil Song, Namho Kim, Namjun Cho

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Properties and compositions of bitumen and bitumen-derived liquids have significant influences on the selection of recovery, upgrading and refining processes. Optimal process conditions can often be directly related to these properties. The end uses of bitumen and bitumen products are thus related to their compositions. Because it is not possible to conduct a complete analysis of the molecular structure of bitumen, characterization must be made in other terms. The present paper focuses on physico-chemical analysis of two different types of bitumens. These bitumen samples were chosen based on: the original crude oil (sand oil and crude petroleum), and mode of process. The aim of this study is to determine both the manufacturing effect on chemical species and the chemical organization as a function of the type of bitumen sample. In order to obtain information on bitumen chemistry, elemental analysis (C, H, N, S, and O), heavy metal (Ni, V) concentrations, IATROSCAN chromatography (thin layer chromatography-flame ionization detection), FTIR spectroscopy, and 1H NMR spectroscopy have all been used. The characterization includes information about the major compound types (saturates, aromatics, resins and asphaltenes) which can be compared with similar data for other bitumens, more importantly, can be correlated with data from petroleum samples for which refining characteristics are known. Examination of Asphalt Ridge froth bitumen showed that it differed significantly from representative petroleum pitches, principally in their nonhydrocarbon content, heavy metal content and aromatic compounds. When possible, properties and composition were related to recovery and refining processes. This information is important because of the effects that composition has on recovery and processing reactions.

Keywords: froth bitumen, oil sand, asphalt ridge, petroleum pitch, thin layer chromatography-flame ionization detection, infrared spectroscopy, 1H nuclear magnetic resonance spectroscopy

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Authors: Liping Wu, Durga Bhakta Pokharel, Junhua Dong, Changgang Wang, Lin Zhao, Wei Ke, Nan Chen

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Hazenite conversion coating was deposited on AZ31 Mg alloy in a deaerated phosphate solution containing 0.1 M K₂HPO₄ and 0.1 M Na₂HPO₄ (Na₀.₁K0₀.₁) with pH 9 at −0.8 V. The coating mechanism of hazenite was elucidated by in situ potentiostatic current decay, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), electron probe micro-analyzer (EPMA) and differential scanning calorimetry (DSC). The volume of H₂ evolved during potentiostatic polarization was measured by a gas collection apparatus. The degradation resistance of the hazenite coating was evaluated in simulated body fluid (SBF) at 37℃ by using potentiodynamic polarization (PDP). The results showed that amorphous Mg(OH)₂ was deposited first, followed by the transformation of Mg(OH)₂ to amorphous MgHPO₄, subsequently the conversion of MgHPO₄ to crystallized K-struvite (KMgPO₄·6H₂O), finally the crystallization of crystallized hazenite (NaKMg₂(PO₄)₂·14H₂O). The deposited coating was composed of four layers where the inner layer is comprised of Mg(OH)₂, the middle layer of Mg(OH)₂ and MgHPO₄, the top layer of Mg(OH)₂, MgHPO₄ and K-struvite, the topmost layer of Mg(OH)₂, MgHPO₄, K-struvite and hazenite (NaKMg₂(PO₄)₂·14H₂O). The PD results showed that the hazenite coating decreased the corrosion rate by two orders of magnitude.

Keywords: magnesium alloy, potentiostatic technique, hazenite, mineral conversion coating

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Authors: Mohamed A. Deyab, Omnia El-Shamy

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The main objective of this case study is to integrate the advantages of cathodic protection technologies in order to lessen chloride-induced corrosion in reinforced concrete. This research employs potentiodynamic polarisation, impedance spectroscopy (EIS), and surface characteristics. The results showed how effectively the new cathodic control strategy is preventing corrosion of the concrete iron rods. Over time, the protective system becomes more reliable and effective. The potentials of the zinc electrode persist still more negative after 30 days, implying that the zinc electrode can maintain powerful electrocatalytic behavior for a long period of time. As per the electrochemical impedance spectroscopy (EIS), using the CP technique reduces the rate of corrosion of rebar iron in cementitious materials over time.

Keywords: cathodic protection, corrosion, reinforced concrete, chloride

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Authors: M. I. Benamrani, H. Benamrani

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In the research to replace silicon and other thin-film semiconductor technologies and to develop long-term technology that is environmentally friendly, low-cost, and abundant, there is growing interest today given to organic materials. Our objective is to prepare polymeric layers containing metal particles deposited on a surface of semiconductor material which can have better electrical properties and which could be applied in the fields of nanotechnology as an alternative to the existing processes involved in the design of electronic circuits. This work consists in the development of composite materials by complexation and electroreduction of copper in a film of poly (pyrrole benzoic acid). The deposition of the polymer film on a monocrystalline silicon substrate is made by electrochemical oxidation in an organic medium. The incorporation of copper particles into the polymer is achieved by dipping the electrode in a solution of copper sulphate to complex the cupric ions, followed by electroreduction in an aqueous solution to precipitate the copper. In order to prepare the monocrystalline silicon substrate as an electrode for electrodeposition, an in-depth study on its surface state was carried out using photoacoustic spectroscopy. An analysis of the optical properties using this technique on the effect of pickling using a chemical solution was carried out. Transmission-photoacoustic and impedance spectroscopic techniques give results in agreement with those of photoacoustic spectroscopy.

Keywords: photoacoustic, spectroscopy, copper sulphate, chemical solution

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Authors: Ljerka Kratofil Krehula, Martina Perlog, Jasmina Stjepanović, Vanja Gilja, Marijana Kraljić Roković, Zlata Hrnjak-Murgić

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The composite preparation of titanium dioxide and zinc oxide photocatalysts with the conductive polymers gives the opportunity to carry out the catalysis reactions not only under UV light but also under visible light. Such processes may efficiently use sunlight in degradation of different organic pollutants and present new design for wastewater treatment. The paper presents the preparation procedure, material characteristics and photocatalytic efficiency of polypyrrole/titanium dioxide and polypyrrole/zinc oxide composites (PPy/TiO2 and PPy/ZnO). The obtained composite samples were characterized by Fourier transform infrared spectroscopy (FTIR), UV-Vis spectroscopy and thermogravimetric analysis (TGA). The photocatalytic efficiency of the samples was determined following the decomposition of Acid Blue 25 dye (AB 25) under UV and visible light by UV/Vis spectroscopy. The efficiency of degradation is determined by total organic carbon content (TOC) after photocatalysis processes. The results show enhanced photocatalytic efficiency of the samples under visible light, so the prepared composite samples are recognized as efficient catalysts in degradation process of AB 25 dye. It can be concluded that the preparation of TiO2 or ZnO composites with PPy can serve as a very efficient method for the improvement of TiO2 and ZnO photocatalytic performance under visible light.

Keywords: composite, photocatalysis, polypyrrole, titanium dioxide, zinc oxide

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Authors: A. Almaneea, N. Kapur, J. L. Summers, H. M. Thompson

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Meeting the growth in demand for digital services such as social media, telecommunications, and business and cloud services requires large scale data centres, which has led to an increase in their end use energy demand. Generally, over 30% of data centre power is consumed by the necessary cooling overhead. Thus energy can be reduced by improving the cooling efficiency. Air and liquid can both be used as cooling media for the data centre. Traditional data centre cooling systems use air, however liquid is recognised as a promising method that can handle the more densely packed data centres. Liquid cooling can be classified into three methods; rack heat exchanger, on-chip heat exchanger and full immersion of the microelectronics. This study quantifies the improvements of heat transfer specifically for the case of immersed microelectronics by varying the CPU and heat sink location. Immersion of the server is achieved by filling the gap between the microelectronics and a water jacket with a dielectric liquid which convects the heat from the CPU to the water jacket on the opposite side. Heat transfer is governed by two physical mechanisms, which is natural convection for the fixed enclosure filled with dielectric liquid and forced convection for the water that is pumped through the water jacket. The model in this study is validated with published numerical and experimental work and shows good agreement with previous work. The results show that the heat transfer performance and Nusselt number (Nu) is improved by 89% by placing the CPU and heat sink on the bottom of the microelectronics enclosure.

Keywords: CPU location, data centre cooling, heat sink in enclosures, immersed microelectronics, turbulent natural convection in enclosures

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Authors: Siti Nurhidayah Naqiah Abdull Rani, Herlina Abdul Rahim

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Near infrared (NIR) spectroscopy has always been of great interest in the food and agriculture industries. The development of predictive models has facilitated the estimation process in recent years. In this research, 176 crude palm oil (CPO) samples acquired from Felda Johor Bulker Sdn Bhd were studied. A FOSS NIRSystem was used to tak e absorbance measurements from the sample. The wavelength range for the spectral measurement is taken at 1600nm to 1900nm. Partial Least Square Regression (PLSR) prediction model with 50 optimal number of principal components was implemented to study the relationship between the measured Free Fatty Acid (FFA) values and the measured spectral absorption. PLSR showed predictive ability of FFA values with correlative coefficient (R) of 0.9808 for the training set and 0.9684 for the testing set.

Keywords: palm oil, fatty acid, NIRS, PLSR

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Authors: Renata Gerhardt, Detlev Belder

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Raman spectroscopy has attracted much attention as a structurally descriptive and label-free detection method. It is particularly suited for chemical analysis given as it is non-destructive and molecules can be identified via the fingerprint region of the spectra. In this work possibilities are investigated how to integrate Raman spectroscopy as a detection method for chip-based chromatography, making use of a droplet interface. A demanding task in lab-on-a-chip applications is the specific and sensitive detection of low concentrated analytes in small volumes. Fluorescence detection is frequently utilized but restricted to fluorescent molecules. Furthermore, no structural information is provided. Another often applied technique is mass spectrometry which enables the identification of molecules based on their mass to charge ratio. Additionally, the obtained fragmentation pattern gives insight into the chemical structure. However, it is only applicable as an end-of-the-line detection because analytes are destroyed during measurements. In contrast to mass spectrometry, Raman spectroscopy can be applied on-chip and substances can be processed further downstream after detection. A major drawback of Raman spectroscopy is the inherent weakness of the Raman signal, which is due to the small cross-sections associated with the scattering process. Enhancement techniques, such as surface enhanced Raman spectroscopy (SERS), are employed to overcome the poor sensitivity even allowing detection on a single molecule level. In SERS measurements, Raman signal intensity is improved by several orders of magnitude if the analyte is in close proximity to nanostructured metal surfaces or nanoparticles. The main gain of lab-on-a-chip technology is the building block-like ability to seamlessly integrate different functionalities, such as synthesis, separation, derivatization and detection on a single device. We intend to utilize this powerful toolbox to realize Raman detection in chip-based chromatography. By interfacing on-chip separations with a droplet generator, the separated analytes are encapsulated into numerous discrete containers. These droplets can then be injected with a silver nanoparticle solution and investigated via Raman spectroscopy. Droplet microfluidics is a sub-discipline of microfluidics which instead of a continuous flow operates with the segmented flow. Segmented flow is created by merging two immiscible phases (usually an aqueous phase and oil) thus forming small discrete volumes of one phase in the carrier phase. The study surveys different chip designs to realize coupling of chip-based chromatography with droplet microfluidics. With regards to maintaining a sufficient flow rate for chromatographic separation and ensuring stable eluent flow over the column different flow rates of eluent and oil phase are tested. Furthermore, the detection of analytes in droplets with surface enhanced Raman spectroscopy is examined. The compartmentalization of separated compounds preserves the analytical resolution since the continuous phase restricts dispersion between the droplets. The droplets are ideal vessels for the insertion of silver colloids thus making use of the surface enhancement effect and improving the sensitivity of the detection. The long-term goal of this work is the first realization of coupling chip based chromatography with droplets microfluidics to employ surface enhanced Raman spectroscopy as means of detection.

Keywords: chip-based separation, chip LC, droplets, Raman spectroscopy, SERS

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Authors: Prakash Chand, Anurag Gaur, Ashavani Kumar

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In the present study, we have synthesized Cr and Fe doped zinc oxide (ZnO) nano-structures (Zn1-δCraFebO; where δ= a + b=20%, a = 5, 6, 8 & 10% and b=15, 14, 12 & 10%) via sol-gel method at different doping concentrations. The synthesized samples were characterized for structural properties by X-ray diffractometer and field emission scanning electron microscope and the optical properties were carried out through photoluminescence and UV-visible spectroscopy. The particle size calculated through field emission scanning electron microscope varies from 41 to 96 nm for the samples synthesized at different doping concentrations. The optical band gaps calculated through UV-visible spectroscopy are found to be decreasing from 3.27 to 3.02 eV as the doping concentration of Cr increases and Fe decreases.

Keywords: nano-structures, optical properties, sol-gel method, zinc oxide

Procedia PDF Downloads 296