Search results for: scanning electrochemical microscopy

Authors: Mahfouz Saeed

Abstract:

Cu₂(ZnSn)(S)₄ (CTZS) offers potential advantages over CuInGaSe₂ (CIGS) as solar thin film because to its higher band gap. Preparing such photovoltaic materials by electrochemical techniques is particularly attractive due to the lower processing cost and the high throughput of such techniques. Several recent publications report CTZS electroplating; however, the electrochemical process still facing serious challenges such as a sulfur atomic ration which is about 50% of the total alloy. We introduce in this work an improved electrolyte composition which enables the direct electrodeposition of CTZS from a single bath. The electrolyte is significantly more dilute in comparison to common baths described in the literature. The bath composition we introduce is: 0.0032 M CuSO₄, 0.0021 M ZnSO₄, 0.0303 M SnCl₂, 0.0038 M Na₂S₂O₃, and 0.3 mM Na₂S₂O3. PHydrion is applied to buffer the electrolyte to pH=2, and 0.7 M LiCl is applied as supporting electrolyte. Electrochemical process was carried at a rotating disk electrode which provides quantitative characterization of the flow (room temperature). Comprehensive electrochemical behavior study at different electrode rotation rates are provided. The effects of agitation on atomic composition of the deposit and its adhesion to the molybdenum back contact are discussed. The post treatment annealing was conducted under sulfur atmosphere with no need for metals addition from the gas phase during annealing. The potential which produced the desired atomic ratio of CTZS at -0.82 V/NHE. Smooth deposit, with uniform composition across the sample surface and depth was obtained at 500 rpm rotation speed. Final sulfur atomic ratio was adjusted to 50.2% in order to have the desired atomic ration. The final composition was investigated using Energy-dispersive X-ray spectroscopy technique (EDS). XRD technique used to analyze CTZS crystallography and thickness. Complete and functional CTZS PV devices were fabricated by depositing all the required layers in the correct order and the desired optical properties. Acknowledgments: Case Western Reserve University for the technical help and for using their instruments.

Keywords: photovoltaic, CTZS, thin film, electrochemical

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Authors: Saifon Chongthub

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The purpose of this research is to synthesize adsorbent foam for CO2 adsorption. The polymer was prepared from poly High Internal Phase Emulsion (PolyHIPE) using styrene as monomer and divinylbenzene as comonomer. Its morphology was determined by Scanning Electron Microscopy (SEM). To further increased CO2 adsorption of the prepared polyHIPE, the layer by layer (LbL) technique was applied, which alternated polyelectrolyte injection between layers of Poly(styrenesulfonate) (PSS) and Poly(diallyldimetyl-ammonium chloride)(PDADMAC) as primary layer, and layers of PSS and polyetyleneimine (PEI) as secondary layer.

Keywords: high internal phase emulsion, polyHIPE, surface modification, layer by layer technique, CO2 adsorption

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Authors: M. K. Manoj, V. Pancholi, S. K. Nath

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Microalloyed dual phase steels have been prepared by intercritical austenitisation (ICA) treatment of normalized steel at different temperature and time. Water quenching wad carried to obtain different martensite volume fraction (MVF) in DP steels. DP steels and normalized steels have been characterized by optical and scanning electron microscopy, Vickers hardness measurements and tensile properties determination. The effect of MVF and martensite morphology on mechanical properties and fracture behavior of microalloyed dual phase steels have been explained in the present work.

Keywords: dual phase steel, martensite morphology, hardness, tensile strength

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Authors: Alvaro Ramírez, Martín Muñoz-Morales, Ester López- Fernández, Javier Llanos, C. Ania

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Carbon blacks are value-added materials typically produced through the incomplete combustion or thermal decomposition of hydrocarbons. Traditionally, they have been used as catalysts in many different applications, but in the last decade, their potential in green chemistry has gained significant attention. Among them, the electrochemical production of H₂O₂ has attracted interest because of their properties as high oxidant capacity or their industrial interest as a bleaching agent. Carbon blacks are commonly used in this application in a catalytic ink that is drop-casted on supporting electrodes and acts as catalysts for the electrochemical production of H₂O₂ through oxygen reduction reaction (ORR). However, the different structural and electrochemical behaviors of each type of carbon black influence their applications. In this line, the term ‘carbon black’, has to be considered as a generic name that does not guarantee any physicochemical properties if any further description is mentioned. In fact, different specific surface area (SSA), surface functional groups, porous structure, and electro catalysts effect seem very important for electrochemical applications, and considerable differences were found during the analysis of four types of carbon blacks. Thus, the aim of this work is to evaluate the influence of SSA, porous structure, oxygen functional groups, and structural defects to differentiate among these carbon blacks (e.g. Vulcan XC72, Superior Graphite Co, Printex XE2, and Prolabo) for H₂O₂ production via ORR, using carbon paper as electrode support with improved selectivity and efficiency. Results indicate that the number and size of pores, along with surface functional groups, are key parameters that significantly affect the overall process efficiency.

Keywords: carbon blacks, oxygen reduction reaction, hydrogen peroxide, porosity, surface functional groups

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Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

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The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

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Authors: Xinyong Li

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A new coupling system was constructed by combining photo-electrochemical cell with eletro-fenton cell (PEC-EF). The electrode material in this system was derived from MnyFe₁₋yCo Prussian-Blue-Analog (PBA). Mn₀.₄Fe₀.₆Co₀.₆₇-N@C spin-coated on carbon paper behaved as the gas diffusion cathode and Mn₀.₄Fe₀.₆Co₀.₆₇O₂.₂ spin-coated on fluorine-tin oxide glass (FTO) as anode. The two separated cells could degrade Sulfamethoxazole (SMX) simultaneously and some coupling mechanisms by PEC and EF enhancing the degradation efficiency were investigated. The continuous on-site generation of H₂O₂ at cathode through an oxygen reduction reaction (ORR) was realized over rotating ring-disk electrode (RRDE). The electron transfer number (n) of the ORR with Mn₀.₄Fe₀.₆Co₀.₆₇-N@C was 2.5 in the selected potential and pH range. The photo-electrochemical properties of Mn₀.₄Fe₀.₆Co₀.₆₇O₂.₂ were systematically studied, which displayed good response towards visible light. The photo-induced electrons at anode can transfer to cathode for further use. Efficient photo-electro-catalytic performance was observed in degrading SMX. Almost 100% SMX removal was achieved in 120 min. This work not only provided a highly effective technique for antibiotic treatment but also revealed the synergic effect between PEC and EF.

Keywords: Electro-Fenton, photo-electrochemical, synergic effect, sulfamethoxazole

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Authors: O. Tovide, N. Jahed, N. Mohammed, C. E. Sunday, H. R. Makelane, R. F. Ajayi, K. M. Molapo, A. Tsegaye, M. Masikini, S. Mailu, A. Baleg, T. Waryo, P. G. Baker, E. I. Iwuoha

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A graphenated–polyaniline (GR-PANI) nanocomposite sensor was constructed and used for the determination of anthracene. The direct electro-oxidation behavior of anthracene on the GR-PANI modified glassy carbon electrode (GCE) was used as the sensing principle. The results indicate thatthe response profile of the oxidation of anthracene on GR-PANI-modified GCE provides for the construction of sensor systems based onamperometric and potentiometric signal transductions. A dynamic linear range of 0.12- 100 µM anthracene and a detection limit of 0.044 µM anthracene were established for the sensor system.

Keywords: electrochemical sensors, environmental pollutants, graphenated-polymers, polyaromatic hydrocarbon

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Authors: Mohamad Syahrizal Ahmad, Illyas M. Isa

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In this paper, a multiwall carbon nanotubes (MWCNT) paste electrode modified by a Zn layered hydroxide-ferulate (ZLH-F) was used for detection of hydroquinone (HQ). The morphology and characteristic of the ZLH-F/MWCNT were investigated by scanning electron microscope (SEM), transmission electron microscope (TEM) and square wave voltammetry (SWV). Under optimal conditions, the SWV response showed linear plot for HQ concentration in the range of 1.0×10⁻⁵ M – 1.0×10⁻³ M. The detection limit was found to be 5.7×10⁻⁶ M and correlation coefficient of 0.9957. The glucose, fructose, sucrose, bisphenol A, acetaminophen, lysine, NO₃⁻, Cl⁻ and SO₄²⁻ did not interfere the HQ response. This modified electrode can be used to determine HQ content in wastewater and cosmetic cream with range of recovery 97.8% - 103.0%.

Keywords: 1, 4-dihydroxybenzene, hydroquinone, multiwall carbon nanotubes, square wave voltammetry

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Authors: Xiaojie Jiang, Wei Cai, Yinxiao Xiang, Ni Zhang, Mengxin Ren, Xinzheng Zhang, Jingjun Xu

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Reflection phase of graphene plasmons (GPs) at an abrupt interface is very important, which determines the plasmon resonance of graphene structures of deep sub-wavelength scales. However, at an abrupt graphene edge, the reflection phase is always a constant, ΦR ≈ π/4. In this work, we show that the reflection phase of GPs can be efficiently changed through substrate design. Reflection phase of graphene plasmons (GPs) at an abrupt interface is very important, which determines the plasmon resonance of graphene structures of deep sub-wavelength scales. However, at an abrupt graphene edge, the reflection phase is always a constant, ΦR ≈ π/4. In this work, we show that the reflection phase of GPs can be efficiently changed through substrate design. Specifically, the reflection phase is no longer π/4 at the interface formed by placing a graphene sheet on different substrates. Moreover, tailorable reflection phase of GPs up to 2π variation can be further achieved by scattering GPs at a junction consisting of two such dielectric interfaces with various gap width acting as a Fabry-Perot cavity. Besides, the evolution of plasmon mode in graphene ribbons based on the interface reflection phase tuning is predicted, which is expected to be observed in near-field experiments with scattering-type scanning near-field optical microscopy (s-SNOM). Our work provides another way for in-plane plasmon control, which should find applications for integrated plasmon devices design using graphene.Specifically, the reflection phase is no longer π/4 at the interface formed by placing a graphene sheet on different substrates. Moreover, tailorable reflection phase of GPs up to 2π variation can be further achieved by scattering GPs at a junction consisting of two such dielectric interfaces with various gap width acting as a Fabry-Perot cavity. Besides, the evolution of plasmon mode in graphene ribbons based on the interface reflection phase tuning is predicted, which is expected to be observed in near-field experiments with scattering-type scanning near-field optical microscopy (s-SNOM). Our work provides a new way for in-plane plasmon control, which should find applications for integrated plasmon devices design using graphene.

Keywords: graphene plasmons, reflection phase tuning, plasmon mode tuning, Fabry-Perot cavity

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Authors: In-Hyuck Song, Jang-Hoon Ha

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Recently, porous ceramic membranes have attracted great interest due to their outstanding thermal and chemical stability. In this paper, we report the results of our efforts to determine whether we could prepare a diatomite-kaolin composite coating to be deposited over a sintered diatomite support layer that could reduce the largest pore size of the sintered diatomite membrane while retaining an acceptable level of permeability. We determined under what conditions such a composite coating over a support layer could be prepared without the generation of micro-cracks during drying and sintering. The pore characteristics of the sintered diatomite membranes were studied by scanning electron microscopy and capillary flow porosimetry.

Keywords: ceramic membrane, diatomite, water treatment, sintering

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Authors: Seyfullah Madakbas, Hatice Birtane, Memet Vezir Kahraman

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In this study, we aimed to synthesize and characterize polyhedral oligomeric silsesquioxanes containing polyimide nanocomposite. Polyimide nanocomposites widely have been used in membranes in fuel cell, solar cell, gas filtration, sensors, aerospace components, printed circuit boards. Firstly, polyamic acid was synthesized and characterized by Fourier Transform Infrared. Then, polyhedral oligomeric silsesquioxanes containing polyimide nanocomposite was prepared with thermal imidization method. The obtained polyimide nanocomposite was characterized by Fourier Transform Infrared, Scanning Electron Microscope, Thermal Gravimetric Analysis and Differential Scanning Calorimetry. Thermal stability of polyimide nanocomposite was evaluated by thermal gravimetric analysis and differential scanning calorimetry. Surface morphology of composite samples was investigated by scanning electron microscope. The obtained results prove that successfully prepared polyhedral oligomeric silsesquioxanes are containing polyimide nanocomposite. The obtained nanocomposite can be used in many industries such as electronics, automotive, aerospace, etc.

Keywords: polyimide, nanocomposite, polyhedral oligomeric silsesquioxanes

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Authors: Fernando G. Torres, Donna M. Ebenstein, Monica Merino

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Most fish are covered by a protective external armour. The characteristics of these armours depend on the individual elements that form them, such as scales, scutes or dermal plates. In this work, we assess the properties of two different types of protective elements: scales from A. gigas and dermal plates from P. pardalis. A. Gigas and P. Pardalis are two Amazonian fish with a rather prehistoric aspect. They have large scales and dermal plates that form two different types of protective body armours. Although both scales and dermal plates are formed by collagen and hydroxyapatite, their structures display remarkable differences. The structure and composition of the samples were assessed by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). Morphology studies were carried out using a Scanning Electron Microscopy (SEM). Nanoindentation tests were performed to measure the reduced moduli in A. gigas scales and P. pardalis plates. The similarities and differences between scales and dermal plates are discussed based on the experimental results. Both protective armours are designed to be lightweight, flexible and tough. A. Gigas scales are are light laminated composites, while P. pardalis dermal plates show a sandwich like structure with dense outer layers and a porous inner matrix. It seems that the armour of P. pardalis is more suited for a bottom-dwelling fish and allows for protection against predators. The scales from A. Gigas are more adapted to give protection to a swimming fish. The information obtained from these studies is also important for the development of bioinspired nanocomposites, with potential applications in the biomedical field.

Keywords: pterygoplichthys pardalis, dermal plates arapaima gigas, fish scales

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Authors: Behnoush Dousti, Ye Choi, Gil S. Lee

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Microsupercapacitors (MScs) are known as the future of miniaturized energy sources that can be coupled to a battery to deliver stable and constant energy to microelectronics. Among all their counterparts, electrochemical microsupercapacitor have drawn the most research attention due to their higher power density and long cycle life. Designing the microstructure and choosing the electroactive materials are two significant factors that greatly affect the performance of the device. Here, we report successful fabrication and characterization of a microsupercapacitor with interdigitated structure based on Carbon nanotube sheets (CNT sheet). Novel structure of highly aligned CNT sheet as the electrode materials which also offers excellent conductivity and large surface area along with doping with nitrogen, enabled us to develop a device with serval order of magnitude higher electrochemical performance than the pristine CNT in aqueous electrolyte including high specific capacitance and rate capabilities and excellent cycle life over 10000 cycles. Geometric parameters such as finger width and gap size were also studied and it was shown the device performance is much depended on them. Results of this study confirms the potential of CNT sheet for future energy storage devices.

Keywords: carbon nanotube, energy storage systems, microsupercapacitor, nitrogen doping

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Authors: Misha Ali, Qayyum Husain, Nida Alam, Masood Ahmad

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Improving the activity and stability of the enzyme is an important aspect in bioremediation processes. Immobilization of enzyme is an efficient approach to amend the properties of biocatalyst required during wastewater treatment. The present study was done to immobilize partially purified ginger peroxidase on amino functionalized silica coated titanium dioxide nanocomposite. Interestingly there was an enhancement in enzyme activity after immobilization on nanosupport which was evident from effectiveness factor (η) value of 1.76. Immobilized enzyme was characterized by transmission electron microscopy, scanning electron microscopy and Fourier transform infrared spectroscopy. Immobilized peroxidase exhibited higher activity in a broad range of pH and temperature as compared to free enzyme. Also, the thermostability of peroxidase was strikingly improved upon immobilization. After six repeated uses, the immobilized peroxidase retained around 62% of its dye decolorization activity. There was a 4 fold increase in Vmax of immobilized peroxidase as compared to free enzyme. Circular dichroism spectroscopy demonstrated conformational changes in the secondary structure of enzyme, a possible reason for the enhanced enzyme activity after immobilization. Immobilized peroxidase was highly efficient in the removal of acid yellow 42 dye in a stirred batch process. Our study shows that this bio-remediating system has remarkable potential for treatment of aromatic pollutants present in wastewater.

Keywords: acid yellow 42, decolorization, ginger peroxidase, immobilization

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Authors: Anjana Jain, S. Jayanth Kumar

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

Keywords: dielectric Properties, PANI, PVDF, smart materials

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Authors: Amirhossein Hasani, Shamin Houshmand Sharifi

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In this work, we investigate humidity sensing behavior of the graphene oxide with porous silicon substrate. By evaporation method, aluminum interdigital electrodes have been deposited onto porous silicon substrate. Then, by drop-casting method graphene oxide solution was deposited onto electrodes. The porous silicon was formed by electrochemical etching. The experimental results showed that using porous silicon substrate, we obtained two times larger sensitivity and response time compared with the results obtained with silicon substrate without porosity.

Keywords: graphene oxide, porous silicon, humidity sensor, electrochemical

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Authors: N. Chahmana, I. Zerroual

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The aim of our work is the contribution to the improvement of the performances of the positive plate of the lead acid battery. For that, we synthesized two varieties of PbO2 used in industry, alpha and beta PbO2 by electrochemical way starting from the not formed industrial plates. We studied the kinetics of reduction of the alpha varieties and PbO2 beta on electrode with microcavity in sulphuric medium. The electrochemical study of the powders of α and β-PbO2 was made by cyclic voltamperometry with sweeping of potential by using a traditional assembly with three electrodes. Values of the coefficient of diffusion of the proton in α and β-PbO2 are respectively equal to 0.498*10-8cm2 /s and 0.793*10-8 cm2 /s. During the cycling of the two varieties of PbO2, we obtain a clear increase in the capacity.

Keywords: lead accumulator, α and β - PbO2, synthesis, kinetics, cyclic voltametry, coefficient of diffusion

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Authors: Michael Regev, Shai Essel, Alexander Katz-Demyanetz

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Magnesium alloys are characterized by good physical properties: They exhibit high strength, are lightweight and have good damping absorption and good thermal and electrical conductivity. Amorphous magnesium alloys, moreover, exhibit higher strength, hardness and a large elastic domain in addition to having excellent corrosion resistance. These above-mentioned advantages make magnesium based metallic glasses attractive for industrial use. Among the various existing magnesium alloys, Mg₆₅Cu₂₅Y₁₀ alloy is known to be one of the best glass formers. In the current study, Mg₆₅Cu₂₅Y₁₀ ribbons were produced by melt spinning, their microstructure was investigated in its as-cast condition, after pressing under 0.5 GPa for 5 minutes under different temperatures - RT, 500C, 1000C, 1500C and 2000C - and after five minute exposure to the above temperatures without pressing. The microstructure was characterized by means of X-ray Diffraction (XRD), Differential Scanning Calorimetry (DSC), High Resolution Scanning Electron Microscope (HRSEM) and High Resolution Transmission Electron Microscopy (HRTEM). XRD and DSC studies showed that the as-cast material had an amorphous character and that the material crystallized during exposure to temperature with or without applying stress. HRTEM revealed that the as-cast Mg65Cu25Y10, although known to be one of the best glass formers, is nano-crystalline rather than amorphous. The current study casts light on the question what an amorphous alloy is and whether there is any clear borderline between amorphous and nano-crystalline alloys.

Keywords: metallic glass, magnesium, melt spinning, amorphous alloys

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Authors: Fares Khalfallah, Zakaria Boumerzoug, Selvarajan Rajakumar, Elhadj Raouache

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The ceramic-aluminum bond is strongly present in industrial tools, due to the need to combine the properties of metals, such as ductility, thermal and electrical conductivity, with ceramic properties like high hardness, corrosion and wear resistance. In recent years, some joining techniques have been developed to achieve a good bonding between these materials such as brazing, diffusion bonding, ultrasonic joining and friction welding. In this work, AA1100 aluminum alloy rods were welded with Alumina 99.9 wt% ceramic rods, by friction welding. The effect of friction pressure on mechanical and structural properties of welded joints was studied. The welding was performed by direct friction welding machine. The welding samples were rotated at a constant rotational speed of 900 rpm, friction time of 4 sec, forging strength of 18 MPa, and forging time of 3 sec. Three different friction pressures were applied to 20, 34 and 45 MPa. The three-point bending test and Vickers microhardness measurements were used to evaluate the strength of the joints and investigate the mechanical properties of the welding area. The microstructure of joints was examined by optical microscopy (OM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The results show that bending strength increased, and then decreased after reaching a maximum value, with increasing friction pressure. The SEM observation shows that the increase in friction pressure led to the appearance of cracks in the microstructure of the interface area, which is decreasing the bending strength of joints.

Keywords: welding of ceramic to aluminum, friction welding, alumina, AA1100 aluminum alloy

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Authors: Getenet Aseged Zeleke

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The aim of this project was to study the synthesis of activated carbon from low-cost animal beef and the characterization of the product obtained. The bone was carbonized in an inert atmosphere at three different temperatures (500°C, 700oC and 900°C) in an electric furnace, followed by activation with hydrochloric acid. The activated animal bone charcoals obtained were characterized by using scanning electron microscopy (SEM)to observe the effect of activation compared to the unactivated bone charcoal. The following parameters were also determined: ash content, moisture content, volatile content, fixed carbon, pH, pore volume and bulk (apparent) density. The characterization result showed that the activated bone charcoal has good properties and is compared favorably with other reference activated carbons.

Keywords: bones, carbonization, activation, characterization, activated carbon

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

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

Keywords: dentistry, Eppawala chlorapatite, hydroxyapatite, orthopedics

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Authors: Sanghamitra Acharya, Suwarna Datar

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Extensive use of digital and smart communication createsprolong expose of unwanted electromagnetic (EM) radiations. This harmful radiation creates not only malfunctioning of nearby electronic gadgets but also severely affects a human being. So, a suitable microwave absorbing material (MAM) becomes a necessary urge in the field of stealth and radar technology. Initially, Aluminum based hexa ferrite was prepared by sol-gel technique and for carbon derived composite was prepared by the simple one port chemical reduction method. Finally, composite films of Poly (Vinylidene) Fluoride (PVDF) are prepared by simple gel casting technique. Present work demands that aluminum-based hexaferrite phase conjugated with graphene in PVDF matrix becomes a suitable candidate both in commercially important X and Ku band. The structural and morphological nature was characterized by X-Ray diffraction (XRD), Field emission-scanning electron microscope (FESEM) and Raman spectra which conforms that 30-40 nm particles are well decorated over graphene sheet. Magnetic force microscopy (MFM) and conducting force microscopy (CFM) study further conforms the magnetic and conducting nature of composite. Finally, shielding effectiveness (SE) of the composite film was studied by using Vector network analyzer (VNA) both in X band and Ku band frequency range and found to be more than 30 dB and 40 dB, respectively. As prepared composite films are excellent microwave absorbers.

Keywords: carbon nanocomposite, microwave absorbing material, electromagnetic shielding, hexaferrite

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Authors: William L. Whitehouse, Louisa H. Y. Lo, Andrew B. Kinghorn, Simon C. C. Shiu, Julian. A. Tanner

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C-reactive protein (CRP) is an acute-phase reactant and sensitive indicator for sepsis and other life-threatening pathologies, including systemic inflammatory response syndrome (SIRS). Currently, clinical turn-around times for established CRP detection methods take between 30 minutes to hours or even days from centralized laboratories. Here, we report the development of an electrochemical biosensor using redox probe-tagged DNA aptamers functionalized onto cheap, commercially available screen-printed electrodes. Binding-induced conformational switching of the CRP-targeting aptamer induces a specific and selective signal-ON event, which enables single-step and reagentless detection of CRP in as little as 1 minute. The aptasensor dynamic range spans 5-1000nM (R=0.97) or 5-500nM (R=0.99) in 50% diluted human serum, with a LOD of 3nM, corresponding to 2-orders of magnitude sensitivity under the clinically relevant cut-off for CRP. The sensor is stable for up to one week and can be reused numerous times, as judged from repeated real-time dosing and dose-response assays. By decoupling binding events from the signal induction mechanism, structure-switching electrochemical aptamer-based sensors (SS-EABs) provide considerable advantages over their adsorption-based counterparts. Our work expands on the retinue of such sensors reported in the literature and is the first instance of an SS-EAB for reagentless CRP detection. We hope this study can inspire further investigations into the suitability of SS-EABs for diagnostics, which will aid translational R&D toward fully realized devices aimed at point-of-care applications or for use more broadly by the public.

Keywords: structure-switching, C-reactive protein, electrochemical, biosensor, aptasensor.

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Authors: S. M. Giripunje, Shikha Jindal

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Zinc sulphide (ZnS) quantum dots (QDs) were synthesized successfully via simple sonochemical method. X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) analysis revealed the average size of QDs of the order of 3.7 nm. The band gap of the QDs was tuned to 5.2 eV by optimizing the synthesis parameters. UV-Vis absorption spectra of ZnS QD confirm the quantum confinement effect. Fourier transform infrared (FTIR) analysis confirmed the formation of single phase ZnS QDs. To fabricate the diode, blend of ZnS QDs and P3HT was prepared and the heterojunction of PEDOT:PSS and the blend was formed by spin coating on indium tin oxide (ITO) coated glass substrate. The diode behaviour of the heterojunction was analysed, wherein the ideality factor was found to be 2.53 with turn on voltage 0.75 V and the barrier height was found to be 1.429 eV. ZnS-Graphene QDs nanocomposite was characterised for the surface morphological study. It was found that the synthesized ZnS QDs appear as quasi spherical particles on the graphene sheets. The average particle size of ZnS-graphene nanocomposite QDs was found to be 8.4 nm. From voltage-current characteristics of ZnS-graphene nanocomposites, it is observed that the conductivity of the composite increases by 10⁴ times the conductivity of ZnS QDs. Thus the addition of graphene QDs in ZnS QDs enhances the mobility of the charge carriers in the composite material. Thus, the graphene QDs, with high specific area for a large interface, high mobility and tunable band gap, show a great potential as an electron-acceptors in photovoltaic devices.

Keywords: graphene, heterojunction, quantum confinement effect, quantum dots(QDs), zinc sulphide(ZnS)

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Authors: Leila Samiee, Amir Yadegari, Saeedeh Tasharrofi

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In the work presented here, nitrogen-doped graphene materials were synthesized and used as metal-free electrocatalysts for oxygen reduction reaction (ORR) under alkaline conditions. Paraphenylenediamine was used as N precursor. The N-doped graphene was synthesized under hydrothermal treatment at 200°C. All the materials have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM) and X-ray photo-electron spectroscopy (XPS). Moreover, for electrochemical evaluation of samples, Rotating Disk electrode (RDE) and Cyclic Voltammetry techniques (CV) were employed. The resulting material exhibits an outstanding catalytic activity for the oxygen reduction reaction (ORR) as well as excellent resistance towards methanol crossover effects, indicating their promising potential as ORR electrocatalysts for alkaline fuel cells.

Keywords: alkaline fuel cell, graphene, metal-free catalyst, paraphenylen diamine

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

Abstract:

Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: green chemistry, 1H-indole, heteroaromatic, organic electrosynthesis

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Authors: Mazaher Yarmohamadi-Vasel, Ali Reza Modarresi-Alama, Sahar Shabzendedara

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Purpose/Objectives: The first purpose was synthesize Poly(N-(sulfophenyl)aniline) nanoflowers (PSANFLs) and Poly(N-(sulfophenyl)aniline) nanofibers/titanium dioxide nanoparticles ((PSANFs/TiO2NPs) by a solid-state mechano-chemical reaction and template-free method and use them in hybrid solar cell. Also, our second aim was to increase the solubility and the processability of conjugated nanomaterials in water through polar functionalized materials. poly[N-(4-sulfophenyl)aniline] is easily soluble in water because of the presence of polar groups of sulfonic acid in the polymer chain. Materials/Methods: Iron (III) chloride hexahydrate (FeCl3∙6H2O) were bought from Merck Millipore Company. Titanium oxide nanoparticles (TiO2, <20 nm, anatase) and Sodium diphenylamine-4-sulfonate (99%) were bought from Sigma-Aldrich Company. Titanium dioxide nanoparticles paste (PST-20T) was prepared from Sharifsolar Co. Conductive glasses coated with indium tin oxide (ITO) were bought from Xinyan Technology Co (China). For the first time we used the solid-state mechano-chemical reaction and template-free method to synthesize Poly(N-(sulfophenyl)aniline) nanoflowers. Moreover, for the first time we used the same technique to synthesize nanocomposite of Poly(N-(sulfophenyl)aniline) nanofibers and titanium dioxide nanoparticles (PSANFs/TiO2NPs) also for the first time this nanocomposite was synthesized. Examining the results of electrochemical calculations energy gap obtained by CV curves and UV–vis spectra demonstrate that PSANFs/TiO2NPs nanocomposite is a p-n type material that can be used in photovoltaic cells. Doctor blade method was used to creat films for three kinds of hybrid solar cells in terms of different patterns like ITO│TiO2NPs│Semiconductor sample│Al. In the following, hybrid photovoltaic cells in bilayer and bulk heterojunction structures were fabricated as ITO│TiO2NPs│PSANFLs│Al and ITO│TiO2NPs│PSANFs /TiO2NPs│Al, respectively. Fourier-transform infrared spectra, field emission scanning electron microscopy (FE-SEM), ultraviolet-visible spectra, cyclic voltammetry (CV) and electrical conductivity were the analysis that used to characterize the synthesized samples. Results and Conclusions: FE-SEM images clearly demonstrate that the morphology of the synthesized samples are nanostructured (nanoflowers and nanofibers). Electrochemical calculations of band gap from CV curves demonstrated that the forbidden band gap of the PSANFLs and PSANFs/TiO2NPs nanocomposite are 2.95 and 2.23 eV, respectively. I–V characteristics of hybrid solar cells and their power conversion efficiency (PCE) under 100 mWcm−2 irradiation (AM 1.5 global conditions) were measured that The PCE of the samples were 0.30 and 0.62%, respectively. At the end, all the results of solar cell analysis were discussed. To sum up, PSANFLs and PSANFLs/TiO2NPs were successfully synthesized by an affordable and straightforward mechanochemical reaction in solid-state under the green condition. The solubility and processability of the synthesized compounds have been improved compared to the previous work. We successfully fabricated hybrid photovoltaic cells of synthesized semiconductor nanostructured polymers and TiO2NPs as different architectures. We believe that the synthesized compounds can open inventive pathways for the development of other Poly(N-(sulfophenyl)aniline based hybrid materials (nanocomposites) proper for preparing new generation solar cells.

Keywords: mechanochemical synthesis, PSANFLs, PSANFs/TiO2NPs, solar cell

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Authors: Maria Sofia Palagonia, Doriano Brogioli, Fabio La Mantia

Abstract:

In the last decade, lithium has become an important raw material in various sectors, in particular for rechargeable batteries. Its production is expected to grow more and more in the future, especially for mobile energy storage and electromobility. Until now it is mostly produced by the evaporation of water from salt lakes, which led to a huge water consumption, a large amount of waste produced and a strong environmental impact. A new, clean and faster electrochemical technique to recover lithium has been recently proposed: electrochemical ion pumping. It consists in capturing lithium ions from a feed solution by intercalation in a lithium-selective material, followed by releasing them into a recovery solution; both steps are driven by the passage of a current. In this work, a new configuration of the electrochemical cell is presented, used to study and optimize the process of the intercalation of lithium ions through the hydrodynamic condition. Lithium Manganese Oxide (LiMn₂O₄) was used as a cathode to intercalate lithium ions selectively during the reduction, while Nickel Hexacyano Ferrate (NiHCF), used as an anode, releases positive ion. The effect of hydrodynamics on the process has been studied by conducting the experiments at various fluxes of the electrolyte through the electrodes, in terms of charge circulated through the cell, captured lithium per unit mass of material and overvoltage. The result shows that flowing the electrolyte inside the cell improves the lithium capture, in particular at low lithium concentration. Indeed, in Atacama feed solution, at 40 mM of lithium, the amount of lithium captured does not increase considerably with the flux of the electrolyte. Instead, when the concentration of the lithium ions is 5 mM, the amount of captured lithium in a single capture cycle increases by increasing the flux, thus leading to the conclusion that the slowest step in the process is the transport of the lithium ion in the liquid phase. Furthermore, an influence of the concentration of other cations in solution on the process performance was observed. In particular, the capturing of the lithium using a different concentration of NaCl together with 5 mM of LiCl was performed, and the results show that the presence of NaCl limits the amount of the captured lithium. Further studies can be performed in order to understand why the full capacity of the material is not reached at the highest flow rate. This is probably due to the porous structure of the material since the liquid phase is likely not affected by the convection flow inside the pores. This work proves that electrochemical ion pumping, with a suitable hydrodynamic design, enables the recovery of lithium from feed solutions at the lower concentration than the sources that are currently exploited, down to 1 mM.

Keywords: desalination battery, electrochemical ion pumping, hydrodynamic, lithium

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Authors: Krasimir Ivanov, Elitsa Kolentsova, Nguyen Nguyen, Alexander Peltekov, Violina Angelova

Abstract:

The nanosized zinc hydroxide nitrate has been recently estimated as perspective foliar fertilizer, which has improved zinc solubility, but low phytotoxicity, in comparison with ZnO and other Zn containing compounds. The main problem is obtaining of stable particles with dimensions less than 100 nm. This work studies the effect of preparation conditions on the chemical compositions and particle size of the zinc hydroxide nitrates, prepared by precipitation. Zn(NO3)2.6H2O and NaOH with concentrations, ranged from 0.2 to 3.2M and the initial OH/Zn ratio from 0.5 to 1.6 were used at temperatures from 20 to 60 °C. All samples were characterized in detail by X-ray diffraction, scanning electron microscopy, differential thermal analysis and ICP. Stability and distribution of the zinc hydroxide nitrate particles were estimated too.

Keywords: zinc hydroxide nitrate, nanoparticles, preparation, foliar fertilizer

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Authors: Merve Küçük, M. Lütfi Öveçoğlu

Abstract:

Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.

Keywords: dip coating, polyester fabrics, sol gel, zinc oxide

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