Search results for: Scanning Tunneling Spectroscopy

Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks

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The structural characterization of silicon nano crystals (SiNCs) have been carried out using transmission electron microscope (TEM) and atomic force microscopy (AFM). SiNCs are crystalline with an average diameter of 65 nm. Erbium trichloride was added to silicon nano crystals using a simple chemical procedure. Erbium is useful in this context because it has a narrow emission band at ⋍1536 nm which corresponds to a standard optical telecommunication wavelength. The optical properties of SiNCs and erbium-mixed SiNCs samples have been characterized using UV-vis spectroscopy, confocal Raman spectroscopy and photoluminescence spectroscopy (PL). SiNCs and erbium-mixed SiNCs samples exhibit an orange PL emission peak at around 595 nm that arise from radiative recombination of Si. Erbium-mixed SiNCs also shows a weak PL emission peak at ⋍1536 nm that attributed to the intra-4f transition in erbium ions. The intensity of the PL peak of Si in erbium-mixed SiNCs is increased in the intensity up to ×3 as compared to pure SiNCs. It was observed that intensity of 1536 nm peak decreased dramatically in the presence of silicon nano crystals and the PL emission peak of silicon nano crystals is increased. Therefore, the resulted data present that the energy transfer from erbium ions to SiNCs due to the chemical mixing method which used in this work.

Keywords: Silicon Nanocrystals (SiNCs), Erbium Ion, photoluminescence, energy transfer

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Authors: Erdinç Vural, Bülent Özdalyan, Serkan Özel

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The four-stroke single cylinder diesel engine has been used in this study, the pistons and valves of the engine have been stabilized, the aluminum oxide (Al₂O₃) in different ratios has been added in the power of zirconium (ZrO₂) magnesium oxide (MgO), and has been coated with the plasma spray method. The pistons and valves of the combustion chamber of the engine are coated with 5 different (ZrO₂ + MgO), (ZrO₂ + MgO + 25% Al₂O₃), (ZrO₂ + MgO + 50% Al₂O₃), (ZrO₂ + MgO + 75% Al₂O₃), (Al₂O₃) sample. The material tests have been made for each of the coated engine parts with the scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) using Cu Kα radiation surface analysis methods. The engine tests have been repeated for each sample in any electric dynamometer in full power 1600 rpm, 2000 rpm, 2400 rpm and 2800 rpm engine speeds. The material analysis and engine tests have shown that the best performance has been performed with (ZrO₂ + MgO + 50% Al₂O₃). Thus, there is no significant change in HC and Smoke emissions, but NOx emission is increased, as the engine improves power, torque, specific fuel consumption and CO emissions in the tests made with sample A3.

Keywords: ceramic coating, material characterization, engine performance, exhaust emissions

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Authors: Salim Ahmed

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Electrocoagulation has proven its effectiveness in industrial effluent treatment by eliminating pollutants, particularly metallic ones. The electrochemical processes that occur at aluminium electrodes give excellent performance. In this work, electrocoagulation tests were carried out on an industrial effluent from an electroplating bath located in Casablanca (Morocco). The aim was to remove chromium and reuse the purified water for other purposes within the company. To this end, we have optimised the operating parameters that affect the efficiency of electrocoagulation, such as electrical voltage, electrode material, stirring speed and distance between electrodes. We also evaluated these parameters. The effect on pH, conductivity, turbidity and chromium concentration. The tests were carried out in a perfectly stirred reactor on an industrial solution rich in chromium. The effluent concentration was 1000 mg/L of Cr6+. Chromium removal efficiency was determined for the following operating conditions: aluminium electrodes, regulated voltage of 6 volts and 12 volts, optimum stirring speed of 600 rpm and distance between electrodes of 2 cm. The sludge produced by electrocoagulation was characterised by X-ray diffractometry, infrared spectroscopy (IR) and scanning electron microscopy (SEM).

Keywords: wastewater, chromium, electrocoagulation, aluminium, aluminium hydroxide

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Authors: G. Balaji, R. Balasundaraprabhu, S. Prasanna, M. D. Kannan, K. Sivakumaran, David Mcilroy

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Copper Zin tin sulphide (Cu2ZnSnS4 or CZTS) is found to be better alternative to Copper Indium gallium diselenide as absorber layers in thin film based solar cells due to the utilisation of earth-abundant materials in the midst of lower toxicity. In the present study, Cu2ZnSnS4 thin films were prepared on soda lime glass using (CuS, ZnS, SnS) targets and were deposited by three different stacking orders, using RF Magnetron sputtering. The substrate temperature was fixed at 300 °C during the depositions. CZTS thin films were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and UV-Vis-NIR spectroscopy. All the samples exhibited X-ray peaks pertaining to (112) kesterite phase of CZTS, along with the presence of a predominant wurtzite CZTS phase. X-ray photoelectron spectroscopy revealed the presence of all the elements in all the samples. The change in stacking order clearly shows that it affects the structural and phase properties of the films. Relative atomic concentrations of Zn, Cu, Sn and S, which are determined by high-resolution XPS core level spectra integrated peak areas revealed that the CZTS films exhibit inhomogeneity in both stoichiometry and elemental composition. Raman spectroscopy studies on the film showed the presence of CZTS phase. The energy band gap of the CZTS thin films was found to be in the range of 1.5 eV to 1.6 eV. The films were then annealed at 450 °C for 5 hrs and it was found that the predominant nature of the X-ray peaks has transformed from Wurtzite to Kesterite phase which is highly desirable for absorber layers in thin film solar cells. The optimized CZTS layer was used as an absorber layer in thin film solar cells. ZnS and CdS were used as buffer layers which in turn prepared by Hot wall epitaxy technique. Gallium doped Zinc oxide was used as a transparent conducting oxide. The solar cell structure Glass/Mo/CZTS/CdS or ZnS/GZO has been fabricated, and solar cell parameters were measured.

Keywords: earth-abundant, Kesterite, RF sputtering, thin film solar cells

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Authors: Karima Bourenane, Aissa Keffous

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In this paper, we present an experimental method on the etching reaction of p-type 6H-SiC, etching that was carried out in HF/K₂Cr₂O₇ solutions. The morphology of the etched surface was examined with varying K₂Cr₂O₇ concentrations, etching time and temperature solution. The surfaces of the etched samples were analyzed using Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and Photoluminescence. The surface morphology of samples etched in HF/K₂Cr₂O₇ is shown to depend on the solution composition and bath temperature. The investigation of the HF/K₂Cr₂O₇ solutions on 6H-SiC surface shows that as K₂Cr₂O₇ concentration increases, the etch rate increases to reach a maximum value at about 0.75 M and then decreases. Similar behavior has been observed when the temperature of the solution is increased. The maximum etch rate is found for 80 °C. Taking into account the result, a polishing etching solution of 6H-SiC has been developed. In addition, the result is very interesting when, to date, no chemical polishing solution has been developed on silicon carbide (SiC). Finally, we have proposed a dissolution mechanism of the silicon carbide in HF/K₂Cr₂O₇ solutions.

Keywords: silicon carbide, dissolution, Chemical etching, mechanism

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Authors: Totsaporn Suwannaruang, Kitirote Wantala

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The purposes of this research were to synthesize titanium dioxide photocatalyst doped with nitrogen (N-doped TiO₂) by hydrothermal method and to test the photocatalytic degradation of paraquat under UV and visible light illumination. The effect of calcination treatment temperature on their physical and chemical properties and photocatalytic efficiencies were also investigated. The characterizations of calcined N-doped TiO₂ photocatalysts such as specific surface area, textural properties, bandgap energy, surface morphology, crystallinity, phase structure, elements and state of charges were investigated by Brunauer, Emmett, Teller (BET) and Barrett, Joyner, Halenda (BJH) equations, UV-Visible diffuse reflectance spectroscopy (UV-Vis-DRS) by using the Kubelka-Munk theory, Wide-angle X-ray scattering (WAXS), Focussed ion beam scanning electron microscopy (FIB-SEM), X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS), respectively. The results showed that the effect of calcination temperature was significant on surface morphology, crystallinity, specific surface area, pore size diameter, bandgap energy and nitrogen content level, but insignificant on phase structure and oxidation state of titanium (Ti) atom. The N-doped TiO₂ samples illustrated only anatase crystalline phase due to nitrogen dopant in TiO₂ restrained the phase transformation from anatase to rutile. The samples presented the nanorice-like morphology. The expansion on the particle was found at 650 and 700°C of calcination temperature, resulting in increased pore size diameter. The bandgap energy was determined by Kubelka-Munk theory to be in the range 3.07-3.18 eV, which appeared slightly lower than anatase standard (3.20 eV), resulting in the nitrogen dopant could modify the optical absorption edge of TiO₂ from UV to visible light region. The nitrogen content was observed at 100, 300 and 400°C only. Also, the nitrogen element disappeared at 500°C onwards. The nitrogen (N) atom can be incorporated in TiO₂ structure with the interstitial site. The uncalcined (100°C) sample displayed the highest percent paraquat degradation under UV and visible light irradiation due to this sample revealed both the highest specific surface area and nitrogen content level. Moreover, percent paraquat removal significantly decreased with increasing calcination treatment temperature. The nitrogen content level in TiO₂ accelerated the rate of reaction with combining the effect of the specific surface area that generated the electrons and holes during illuminated with light. Therefore, the specific surface area and nitrogen content level demonstrated the important roles in the photocatalytic activity of paraquat under UV and visible light illumination.

Keywords: restraining phase transformation, interstitial site, chemical charge state, photocatalysis, paraquat degradation

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Authors: M. Bodner, M. Scampicchio

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Fourier Transform Infrared (FT-IR) spectroscopy coupled with chemometrics was used to distinguish between butter samples and non-butter samples. Further, quantification of the content of margarine in adulterated butter samples was investigated. Fingerprinting region (1400-800 cm^–1) was used to develop unsupervised pattern recognition (Principal Component Analysis, PCA), supervised modeling (Soft Independent Modelling by Class Analogy, SIMCA), classification (Partial Least Squares Discriminant Analysis, PLS-DA) and regression (Partial Least Squares Regression, PLS-R) models. PCA of the fingerprinting region shows a clustering of the two sample types. All samples were classified in their rightful class by SIMCA approach; however, nine adulterated samples (between 1% and 30% w/w of margarine) were classified as belonging both at the butter class and at the non-butter one. In the two-class PLS-DA model’s (R² = 0.73, RMSEP, Root Mean Square Error of Prediction = 0.26% w/w) sensitivity was 71.4% and Positive Predictive Value (PPV) 100%. Its threshold was calculated at 7% w/w of margarine in adulterated butter samples. Finally, PLS-R model (R² = 0.84, RMSEP = 16.54%) was developed. PLS-DA was a suitable classification tool and PLS-R a proper quantification approach. Results demonstrate that FT-IR spectroscopy combined with PLS-R can be used as a rapid, simple and safe method to identify pure butter samples from adulterated ones and to determine the grade of adulteration of margarine in butter samples.

Keywords: adulterated butter, margarine, PCA, PLS-DA, PLS-R, SIMCA

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Authors: J. Belovickis, V. Samulionis, J. Banys, M. V. Silibin, A. V. Solnyshkin, A. V. Sysa

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Ferroelectric polymers exhibit good flexibility, processability and low cost of production. Doping of ferroelectric polymers with nanofillers may modify its dielectric, elastic or piezoelectric properties. Carbon nanotubes are one of the ingredients that can improve the mechanical properties of polymer based composites. In this work, we report on both the ultrasonic and the dielectric properties of the copolymer polyvinylidene fluoride/tetrafluoroethylene (P(VDF-TrFE)) of the composition 70/30 mol% with various concentrations of carbon nanotubes (CNT). Experimental study of ultrasonic wave attenuation and velocity in these composites has been performed over wide temperature range (100 K – 410 K) using an ultrasonic automatic pulse-echo tecnique. The temperature dependences of ultrasonic velocity and attenuation showed anomalies attributed to the glass transition and paraelectric-ferroelectric phase transition. Our investigations showed mechanical losses to be dependent on the volume fraction of the CNTs within the composites. The existence of broad hysteresis of the ultrasonic wave attenuation and velocity within the nanocomposites is presented between cooling and heating cycles. By the means of dielectric spectroscopy, it is shown that the dielectric properties may be tuned by varying the volume fraction of the CNT fillers.

Keywords: carbon nanotubes, polymer composites, PVDF-TrFE, ultrasonic spectroscopy

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Authors: Faezeh Shalchy

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Concrete is the most used materials in the world. It is also one of the most versatile while complex materials which human have used for construction. However, concrete is weak in tension, over the past thirty years many studies were accomplished to improve the tensile properties of concrete (cement-based materials) using a variety of methods. One of the most successful attempts is to use polymeric fibers in the structure of concrete to obtain a composite with high tensile strength and ductility. Understanding the mechanical behavior of fiber reinforced concrete requires the knowledge of the fiber/matrix interfaces at the small scale. In this study, a combination of numerical simulations and experimental techniques have been used to study the nano structure of fiber/matrix interfaces. A new model for calcium-silicate-hydrate (C-S-H)/fiber interfaces is proposed based on Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) analysis. The adhesion energy between the C-S-H gel and 2 different polymeric fibers (polyvinyl alcohol and polypropylene) was numerically studied at the atomistic level since adhesion is one of the key factors in the design of fiber reinforced composites. The mechanisms of adhesion as a function of the nano structure of fiber/matrix interfaces are also studied and discussed.

Keywords: fiber-reinforced concrete, adhesion, molecular modeling

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Authors: Mohamed Khalifa Zayet, Salma Belal Eiid, Mushira Mohamed Dahaba

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Introduction: Malignant tumors may not be easily detected by traditional radiographic techniques especially in an anatomically complex area like maxillofacial region. At the same time, the advent of biological functional MRI was a significant footstep in the diagnostic imaging field. Objective: The purpose of this study was to define the malignant metabolic profile of maxillofacial lesions using diffusion MRI and magnetic resonance spectroscopy, as adjunctive aids for diagnosing of such lesions. Subjects and Methods: Twenty-one patients with twenty-two lesions were enrolled in this study. Both morphological and functional MRI scans were performed, where T1, T2 weighted images, diffusion-weighted MRI with four apparent diffusion coefficient (ADC) maps were constructed for analysis, and magnetic resonance spectroscopy with qualitative and semi-quantitative analyses of choline and lactate peaks were applied. Then, all patients underwent incisional or excisional biopsies within two weeks from MR scans. Results: Statistical analysis revealed that not all the parameters had the same diagnostic performance, where lactate had the highest areas under the curve (AUC) of 0.9 and choline was the lowest with insignificant diagnostic value. The best cut-off value suggested for lactate was 0.125, where any lesion above this value is supposed to be malignant with 90 % sensitivity and 83.3 % specificity. Despite that ADC maps had comparable AUCs still, the statistical measure that had the final say was the interpretation of likelihood ratio. As expected, lactate again showed the best combination of positive and negative likelihood ratios, whereas for the maps, ADC map with 500 and 1000 b-values showed the best realistic combination of likelihood ratios, however, with lower sensitivity and specificity than lactate. Conclusion: Diffusion weighted imaging and magnetic resonance spectroscopy are state-of-art in the diagnostic arena and they manifested themselves as key players in the differentiation process of orofacial tumors. The complete biological profile of malignancy can be decoded as low ADC values, high choline and/or high lactate, whereas that of benign entities can be translated as high ADC values, low choline and no lactate.

Keywords: diffusion magnetic resonance imaging, magnetic resonance spectroscopy, malignant tumors, maxillofacial

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Authors: Sergey A. Burikov, Tatiana A. Dolenko, Kirill A. Gushchin, Sergey A. Dolenko

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The paper presents the results of clusterization by Kohonen self-organizing maps (SOM) applied for analysis of array of Raman spectra of multi-component solutions of inorganic salts, for determination of types of salts present in the solution. It is demonstrated that use of SOM is a promising method for solution of clusterization and classification problems in spectroscopy of multi-component objects, as attributing a pattern to some cluster may be used for recognition of component composition of the object.

Keywords: Kohonen self-organizing maps, clusterization, multi-component solutions, Raman spectroscopy

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Authors: Riffat Kalsoom, Qurat-Ul-Ain Javed

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Optical and dielectric properties of lithium niobates have made them the fascinating materials to be used in optical industry for device formation such as Q and optical switching. Synthesis of lithium niobates was carried out by solvothermal process with and without temperature fluctuation at 200°C for 4 hrs, and behavior of properties for different durations was also examined. Prepared samples of LiNbO₃ were examined in a way as crystallographic phases by using XRD diffractometer, morphology by scanning electron microscope (SEM), absorption by UV-Visible Spectroscopy and dielectric measurement by impedance analyzer. A structural change from trigonal to spherical shape was observed by changing the time of reaction. Crystallite size decreases by the temperature fluctuation and increasing reaction time. Band gap decreases whereas dielectric constant and dielectric loss was increased with increasing time of reaction. Trend of AC conductivity is explained by Joschner’s power law. Due to these significant properties, it finds its applications in devices, such as cells, Q switching and optical switching for laser and gigahertz frequencies, respectively and these applications depend on the industrial demands.

Keywords: lithium niobates, renewable energy devices, controlled structure, temperature fluctuations

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Authors: Daniela Ailincai, Bogdan C. Simionescu, Luminita Marin

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Polymer dispersed liquid crystals (PDLC) represent an interesting class of materials which combine the ability of polymers to form films and their mechanical strength with the opto-electronic properties of liquid crystals. The proper choice of the two components - the liquid crystal and the polymeric matrix - leads to materials suitable for a large area of applications, from electronics to biomedical devices. The objective of our work was to obtain PDLC films with potential applications in the biomedical field, using poly vinyl alcohol boric acid (PVAB) as a polymeric matrix for the first time. Presenting all the tremendous properties of poly vinyl alcohol (such as: biocompatibility, biodegradability, water solubility, good chemical stability and film forming ability), PVAB brings the advantage of containing the electron deficient boron atom, and due to this, it should promote the liquid crystal anchoring and a narrow liquid crystal droplets polydispersity. Two different PDLC systems have been obtained, by the use of two liquid crystals, a nematic commercial one: 4-cyano-4’-penthylbiphenyl (5CB) and a new smectic liquid crystal, synthesized by us: buthyl-p-[p’-n-octyloxy benzoyloxy] benzoate (BBO). The PDLC composites have been obtained by the encapsulation method, working with four different ratios between the polymeric matrix and the liquid crystal, from 60:40 to 90:10. In all cases, the composites were able to form free standing, flexible films. Polarized light microscopy, scanning electron microscopy, differential scanning calorimetry, RAMAN- spectroscopy and the contact angle measurements have been performed, in order to characterize the new composites. The new smectic liquid crystal has been characterized using 1H-NMR and single crystal X-ray diffraction and its thermotropic behavior has been established using differential scanning calorimetry and polarized light microscopy. The polarized light microscopy evidenced the formation of round birefringent droplets, anchored homeotropic in the first case and planar in the second, with a narrow dimensional polydispersity, especially for the PDLC containing the largest amount of liquid crystal, fact evidenced by SEM, also. The obtained values for the water to air contact angle showed that the composites have a proper hydrophilic-hydrophobic balance, making them potential candidates for bioapplications. More than this, our studies demonstrated that the water to air contact angle varies as a function of PVAB matrix crystalinity degree, which can be controled as a function of time. This fact allowed us to conclude that the use of PVAB as matrix for PDLCs obtaining offers the possibility to modulate their properties for specific applications.

Keywords: 4-cyano-4’-penthylbiphenyl, buthyl-p-[p’-n-octyloxy benzoyloxy] benzoate, contact angle, polymer dispersed liquid crystals, poly vinyl alcohol boric acid

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Authors: Fatma Gülden Şi̇mşek, Osman Meli̇h Can, Mehmet Yumak, Bora Gari̇pcan, Yekta Ülgen

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In this study, the impedance spectroscopy is used as a detection tool in order to characterize surface coating with graphene oxide. Gold electrodes are produced by standard lithography procedures and then coated with graphene oxide using self-assembly method. The impedance of redox solution through bare gold electrodes and graphene oxide coated gold electrodes is measured in the low and high frequency range. The graphene oxide coating reduces the impedance value of the gold electrode and this reduction is distinguishable in the low-frequency range.

Keywords: bioimpedance, electrode characterization, graphene oxide, gold electrodes, impedance spectroscopy

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Authors: Amit Keshav

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Waste bone, produced in large quantity (8-10 kg./day) from a slaughterhouse, could be a cheap (cost $0.20 per kg) substitute for commercial catalysts. In the present work, catalyst for esterification reaction was prepared from waste bone and characterized by various techniques. Bone was deoiled and then sulfonated. Fourier-transform infrared spectroscopy (FTIR) spectra of prepared catalyst predicted –OH vibration at 3416 and 1630 cm⁻¹, S-O stretching at 1124 cm⁻¹ and intense bands of hydroxypatite in a region between 500 and 700 cm⁻¹. X-ray diffraction (XRD) predicts peaks of hydroxyapatite, CaO, and tricalcium phosphate. Scanning electron microscope (SEM) was employed to reveal the presence of non-uniformity deposited fine particles on the catalyst surface that represents active acidic sites. The prepared catalyst was employed to study its performance on esterification reaction between acrylic acid and ethanol in a molar ratio of 1:1 at a set temperature of 60 °C. Results show an equilibrium conversion of 49% which is matched to the commercial catalysts employed in literature. Thus waste bone could be a good catalyst for acrylic acid removal from waste industrial streams via the process of esterification.Keywords— Heterogeneous catalyst, characterization, esterification, equilibrium conversion

Keywords: heterogeneous catalyst, characterization, esterification, equilibrium conversion

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Authors: Bodhayan Nandi, Shubhajit Roy Chowdhury

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This paper presents the development of a portable blood glucose monitoring device based on Near-Infrared Spectroscopy. The system supports Internet connectivity through WiFi and uploads the time series data of glucose concentration of patients to a server. In addition, the server is given sufficient intelligence to predict the future pathophysiological state of a patient given the current and past pathophysiological data. This will enable to prognosticate the approaching critical condition of the patient much before the critical condition actually occurs.The server hosts web applications to allow authorized users to monitor the data remotely.

Keywords: non invasive, blood glucose concentration, microcontroller, IoT, application server, database server

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Authors: D. V. S. Praneeth, V. R. Sankar Cheela, Brajesh Dubey

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Coal Combustion (CC) residues are the major by-products from thermal power plants. The disposal of ash on to land creates havoc to environment and humans. The leaching of the constituent elements pollutes ground water. Beneficiary use of coal combustion residues in structural components is being investigated as a part of this study. This application reduces stress on the convention materials in the construction industry. The present study involves determination of leaching parameters of the CC residues. Batch and column studies are performed based on Leaching Environmental Assessment Framework (LEAF) protocol. The column studies are conducted to simulate the real time percolation conditions in the field. The structural and environmental studies are performed to determine the usability of CC residues as bricks. The physical, chemical, geo environmental and mechanical properties of the alternate materials are investigated. Scanning electron microscopy (SEM), X-Ray Diffraction analysis (XRD), X-ray fluorescence (XRF) and Energy Dispersive X-ray Spectroscopy tests were conducted to determine the characteristics of CC residue ash and bricks.

Keywords: coal combustion residues, LEAF, leaching, SEM

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Authors: Gichun Cha, Byoungjoon Yu, Jihwan Park, Minsoo Park, Junghyun Im, Sehwan Park, Sujung Sin, Seunghee Park

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The goal of this research is to estimate a structural shape change using terrestrial laser scanning. This study proceeds with development of data reduction and shape change estimation algorithm for large-capacity scan data. The point cloud of scan data was converted to voxel and sampled. Technique of shape estimation is studied to detect changes in structure patterns, such as skyscrapers, bridges, and tunnels based on large point cloud data. The point cloud analysis applies the octree data structure to speed up the post-processing process for change detection. The point cloud data is the relative representative value of shape information, and it used as a model for detecting point cloud changes in a data structure. Shape estimation model is to develop a technology that can detect not only normal but also immediate structural changes in the event of disasters such as earthquakes, typhoons, and fires, thereby preventing major accidents caused by aging and disasters. The study will be expected to improve the efficiency of structural health monitoring and maintenance.

Keywords: terrestrial laser scanning, point cloud, shape information model, displacement measurement

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Authors: P. Hari Prasad Reddy, C. H. Rama Vara Prasad, G. Kalyan Kumar

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This paper presents the morphological and mineralogical changes occurring in the soil due to immediate and prolonged interaction with different concentrations of phosphoric acid and sulphuric acid. In order to assess the effect of acid contamination, a series of sediment volume, scanning electron microscopy and X-ray diffraction analysis tests were carried out on soil samples were exposed to different concentrations (1N, 4N and 8N) of phosphoric and sulphuric acid. Experimental results show that both acids showed severe morphological and mineralogical changes with synthesis of neogenic formations mainly at higher concentrations (4N and 8N) and at prolonged duration of interaction (28 and 80 days).

Keywords: phosphoric acid, scanning electron microscopy, sulphuric acid, x-ray diffraction analysis

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Authors: Ahmed Metawea, Rodrigo Soto, Majeida Kharejesh, Gavin Walker, Ahmad B. Albadarin

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In this study, towards a green approach, we have investigated the effect of operating conditions of solvent assessed twin-screw extruder (TSE) for the production of 4, 4-bipyridine (1-dimensional coordinated polymer (1D)) based coordinated polymer using cobalt nitrate as a metal precursor with molar ratio 1:1. Different operating parameters such as solvent percentage, screw speed and feeding rate are considered. The resultant product is characterized using offline characterization methods, namely Powder X-ray diffraction (PXRD), Raman spectroscopy and scanning electron microscope (SEM) in order to investigate the product purity and surface morphology. A lower feeding rate increased the product’s quality as more resident time was provided for the reaction to take place. The most important influencing factor was the amount of liquid added. The addition of water helped in facilitating the reaction inside the TSE by increasing the surface area of the reaction for particles

Keywords: MOFS, multivariate analysis, process optimization, chemometric

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Authors: Omaima G. Allam, O. A. Hakeim, K. Haggag, N. S. Elshemy

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In the midst of the two decades the use of microwave dielectric warming in the field of science has transformed into a powerful methodology to redesign compound procedures. The potential benefit of the application of these modern methods of treatment emphasize so as to reach to optimum treatment conditions and the best results, especially hydrophobicity, moisture content and increase dyeing processing while maintaining the physical and chemical properties of each textile. Moreover, polyester fibres are sometimes spun together with natural fibres to produce a cloth with blended properties. So that at the present task, the polyester/viscose mix fabrics (60 /40) were pretreated with 4 g/l of KOH for 2 min in microwave irradiation with a liquor ratio 1:25. Subsequently fabrics were inundated with different concentrations of sericin (10, 30, 50 g/l). Treated fabrics were coloured with the commercial dyes samples: Reactive Red 84(Dye 1). C. I. Acid Blue 203(Dye 2) and C.I. Reactive violet 5 (Dye 3). Colour value was specified as well as fastness properties. Likewise, the physical properties of untreated and treated fabrics such as moisture content %, tensile strength, elongation % and were evaluated. The untreated and treated fabrics are described by infrared spectroscopy (FTIR) and scanning electron microscopy.

Keywords: polyester viscose blends fabric, sericin, dyes, colour value

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Authors: Mohamed Izzharif Abdul Halim, Niamh Nic Daeid

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Determining the source of pen inks used on a variety of documents is impartial for forensic document examiners. The examination of inks is often performed to differentiate between inks in order to evaluate the authenticity of a document. A ballpoint pen ink consists of synthetic dyes in (acidic and/or basic), pigments (organic and/or inorganic) and a range of additives. Inks of similar color may consist of different composition and are frequently the subjects of forensic examinations. This study emphasizes on blue ballpoint pen inks available in the market because it is reported that approximately 80% of questioned documents analysis involving ballpoint pen ink. Analytical techniques such as thin layer chromatography, high-performance liquid chromatography, UV-vis spectroscopy, luminescence spectroscopy and infrared spectroscopy have been used in the analysis of ink samples. In this study, application of Diamond Attenuated Total Reflectance (ATR) FTIR is straightforward but preferable in forensic science as it offers no sample preparation and minimal analysis time. The data obtained from these techniques were further analyzed using multivariate chemometric methods which enable extraction of more information based on the similarities and differences among samples in a dataset. It was indicated that some pens from the same manufactures can be similar in composition, however, discrete types can be significantly different.

Keywords: ATR FTIR, ballpoint, multivariate chemometric, PCA

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

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

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

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Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: Tshaiya Devi Thandauthapani, Adam J. Reeve, Adam S. Long, Ian J. Turner, James S. Sharp

Abstract:

Fingermarks are a crucial form of evidence for identifying a person at a crime scene. However, visualising latent (hidden) fingermarks can be difficult, and the correct choice of techniques is essential to develop and preserve any fingermarks that might be present. Knives, firearms and other metal weapons have proven to be challenging substrates (stainless steel in particular) from which to reliably obtain fingermarks. In this study, time of flight secondary ion mass spectroscopy (ToF-SIMS) was used to image fingermarks on metal surfaces. This technique was compared to a conventional superglue based fuming technique that was accompanied by a series of contrast enhancing dyes (basic yellow 40 (BY40), crystal violet (CV) and Sudan black (SB)) on three different metal surfaces. The conventional techniques showed little to no evidence of fingermarks being present on the metal surfaces after a few days. However, ToF-SIMS images revealed fingermarks on the same and similar substrates with an exceptional level of detail demonstrating clear ridge definition as well as detail about sweat pore position and shape, that persist for over 26 days after deposition when the samples were stored under ambient conditions.

Keywords: conventional techniques, latent fingermarks, metal substrates, time of flight secondary ion mass spectroscopy

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Authors: Fakhreldin O. Suliman, Alia H. Al-Battashi

Abstract:

This work explored the interaction of three different imidazoline drugs, naphazoline nitrate (NPH), oxymetazoline hydrochloride (OXY) and xylometazoline hydrochloride (XYL) with two different synthesized cucurbit[n]urils CB[n], cucurbit[7]uril (CB[7]) and cucuribit[8]uril (CB[8]). Three binary inclusion complexes have been investigated in solution and in the solid state. The solid complexes were obtained by lyophilization, whereas the physical mixtures of guests and hosts at a stoichiometric ratio of 1:1 were obtained for each drug. 1HNMR, electrospray ionization mass spectrometry (ESI-MS), and matrix-assisted laser desorption-ionization time-of-flight (MALDI-TOF) mass spectrometry was used to study the complexes prepared in aqueous media. The lyophilized solid complexes were characterized by Fourier transform-infrared spectroscopy (FT-IR), powder X-ray diffractometry (PXRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). MS, FT-IR and PXRD experimental results established in this work reveal that NPH, OXY and XYL molecules form stable inclusion complexes with the two hosts. The TGA and DSC confirmed the enhancement of the thermal stability of each drug and the production of a thermally stable solid complex. The 1HNMR has shown that the protons of the guests faced shifting in ppm and broadening of their peaks upon the formation of inclusion complexes with the selected CB[n]. The aromatic protons of the guest exhibited the highest changes in the chemical shifts and shape of the NMR peaks, suggesting their inclusion into the cavity of the CB[n]. The diffusion coefficients (D), developed from the diffusion-controlled NMR Spectroscopy (DOSY) measurements, for the complexation of the selected imidazoline drugs with CB[7] and CB[8], were decreased in the presence of hosts compared to the free guests indicating the formation of the guest-host adduct. Furthermore, we conducted molecular dynamic simulations and quantum mechanics calculations on these complexes. The results of the theoretical study corroborate the experimental findings and have also shed light on the mechanism of inclusion of the guests into the two hosts. This study generates initial data for potential drug delivery or drug formulation systems for these three selected imidazoline drug compounds based on their inclusion into the CB[n] cavities.

Keywords: cucurbit[n]urils, imidazoline, inclusion complexes, molecular dynamics, DFT calculations, mass spectrometry

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Authors: N. Ammouchi

Abstract:

We have studied the effect of milling time on the structural and hyperfine properties of Ni45Al45Fe10 compound elaborated by mechanical alloying. The elaboration was performed by using the planetary ball mill at different milling times. The as milled powders were characterized by X-ray diffraction (XRD) and Mӧssbauer spectroscopy. From XRD diffraction spectra, we show that the β NiAl(Fe) was completely formed after 24 h of milling time. When the milling time increases, the lattice parameter increases, whereas the grain size decreases to a few nanometres and the mean level of microstrains increases. The analysis of Mӧssbauer spectra indicates that, in addition to a ferromagnetic phase, α-Fe, a paramagnetic disordered phase Ni Al (Fe) solid solution is observed after 2h and only this phase is present after 12h.

Keywords: NiAlFe, nanostructured powders, X-ray diffraction, Mӧssbauer spectroscopy

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Authors: Vivek Kumar, Alexander M. Zaitsev

Abstract:

A study on chemical sensing properties of carbon nanofilms on diamond for developing all-carbon chemical sensors is presented. The films were obtained by high temperature graphitization of diamond followed by successive plasma etchings. Characterization of the films was done by Raman spectroscopy, atomic force microscopy, and electrical measurements. Fast and selective response to common organic vapors as seen as sensitivity of electrical conductance was observed. The phenomenological description of the chemical sensitivity is proposed as a function of the surface and bulk material properties of the films.

Keywords: chemical sensor, carbon nanofilm, graphitization of diamond, plasma etching, Raman spectroscopy, atomic force microscopy

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Authors: Pajaree Donkhampa, Fuangfa Unob

Abstract:

Ceftazidime is an antibiotic drug commonly used to treat several human and veterinary infections. However, the presence of ceftazidime residues in the environment may induce microbial resistance and cause side effects to humans. Therefore, monitoring the level of ceftazidime in environmental resources is important. In this work, a melamine foam platform was proposed for simultaneous extraction and colorimetric detection of ceftazidime based on the azo dye formation on the surface. The melamine foam was chemically modified with polyethyleneimine (PEI) and characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Ceftazidime is a sample that was extracted on the PEI-modified melamine foam and further reacted with nitrite in an acidic medium to form an intermediate diazonium ion. The diazotized molecule underwent an azo coupling reaction with chromotropic acid to generate a red-colored compound. The material color changed from pale yellow to pink depending on the ceftazidime concentration. The photo of the obtained material was taken by a smartphone camera and the color intensity was determined by Image J software. The material fabrication and ceftazidime extraction and detection procedures were optimized. The detection of a sub-ppm level of ceftazidime was achieved without using a complex analytical instrument.

Keywords: colorimetric detection, ceftazidime, melamine foam, extraction, azo dye

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Authors: Guo Lei, Wang Yue, Nakamura Yoshio, Shi Ji

Abstract:

Recently, perpendicular exchange bias (PEB) is introduced as an active topic attracting continuous efforts. Since its discovery, extrinsic control of PEB has been proposed, due to its scientific significance in spintronic devices and potential application in high density magnetic random access memory with perpendicular magnetic tunneling junction (p-MTJ). To our knowledge, the researches aiming to controlling PEB so far are focused mainly on enhancing the interfacial exchange coupling by adjusting the FM/AFM interface roughness, or optimizing the crystalline structures of FM or AFM layer by employing different seed layers. In present work, the effects of magnetoelastically induced PMA on PEB have been explored in [CoO5nm/CoPt5nm]5 multilayer films. We find the PMA strength of FM layer also plays an important role on PEB at the FM/AFM interface and it is effective to control PEB of [CoO5nm/CoPt5nm]5 multilayer films by changing the magnetoelastically induced PMA of CoPt layer. [CoO5nm/CoPt5nm]5 multilayer films were deposited by magnetron sputtering on fused quartz substrate at room temperature, then annealed at 100°C, 250°C, 300°C and 375°C for 3h, respectively. XRD results reveal that all the samples are well crystallized with preferred fcc CoPt (111) orientation. The continuous multilayer structure with sharp component transition at the CoO5nm/CoPt5nm interface are identified clearly by transmission electron microscopy (TEM), x-ray reflectivity (XRR) and atomic force microscope (AFM). CoPt layer in-plane tensile stress is calculated by sin2φ method, and we find it increases gradually upon annealing from 0.99 GPa (as-deposited) up to 3.02 GPa (300oC-annealed). As to the magnetic property, significant enhancement of PMA is achieved in [CoO5nm/CoPt5nm]5 multilayer films after annealing due to the increase of CoPt layer in-plane tensile stress. With the enhancement of magnetoelastically induced PMA, great improvement of PEB is also achieved in [CoO5nm/CoPt5nm]5 multilayer films, which increases from 130 Oe (as-deposited) up to 1060 Oe (300oC-annealed), showing the same change tendency as PMA and the strong correlation with CoPt layer in-plane tensile stress. We consider it is the increase of CoPt layer in-plane tensile stress that leads to the enhancement of PMA, and thus the enhancement of magnetoelastically induced PMA results in the improvement of PEB in [CoO5nm/CoPt5nm]5 multilayer films.

Keywords: perpendicular exchange bias, magnetoelastically induced perpendicular magnetic anisotropy, CoO5nm/CoPt5nm]5 multilayer film with in-plane stress, perpendicular magnetic tunneling junction

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