Search results for: broadband dielectric spectroscopy

Authors: Mahdi Almaky, Reda Hassanin, Benjamin Horrocks, Andrew Houlton

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DNA-templated poly(N-substituted pyrrole)bipyridinium nanowires were synthesised at room temperature using the chemical oxidation method. The resulting CPs/DNA hybrids have been characterised using electronic and vibrational spectroscopic methods especially Ultraviolet-Visible (UV-Vis) spectroscopy and FTIR spectroscpy. The nanowires morphology was characterised using Atomic Force Microscopy (AFM). The electrical properties of the prepared nanowires were characterised using Electrostatic Force Microscopy (EFM), and measured using conductive AFM (c-AFM) and two terminal I/V technique, where the temperature dependence of the conductivity was probed. The conductivities of the prepared CPs/DNA nanowires are generally lower than PPy/DNA nanowires showingthe large effect on N-alkylation in decreasing the conductivity of the polymer, butthese are higher than the conductivity of their corresponding bulk films.This enhancement in conductivity could be attributed to the ordering of the polymer chains on DNA during the templating process. The prepared CPs/DNA nanowires were used as templates for the growth of copper nanowires at room temperature using aqueous solution of Cu(NO3)2as a source of Cu2+ and ascorbic acid as reducing agent. AFM images showed that these nanowires were uniform and continuous compared to copper nanowires prepared using the templating method directly onto DNA. Electrical characterization of the nanowires by c AFM revealed slight improvement in conductivity of these nanowires (Cu-CPs/DNA) compared to CPs/DNA nanowires before metallisation.

Keywords: templating, copper nanowires, polymer/DNA hybrid, chemical oxidation method

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Authors: Silviya Todorova, Anton Naydenov, Ralitsa Velinova, Alexander Larin

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Catalytic combustion of methane has been extensively investigated for emission control and power generation during the last decades. The alumina-supported palladium catalyst is widely accepted as the most active catalysts for catalytic combustion of methane. The activity of Pd/Al₂O₃ decreases during the time on stream, especially underwater vapor. The following order of activity in the reaction of complete oxidation of methane was established: Co₃O₄> CuO>NiO> Mn₂O₃> Cr₂O₃. It may be expected that the combination between Pd and these oxides could lead to the promising catalysts in the reaction of complete methane. In the present work, we investigate the activity of Pd/Al₂O₃ catalysts promoted with other metal oxides (MOx; M= Ni, Co, Ce). The Pd-based catalysts modified by metal oxide were prepared by sequential impregnation of Al₂O₃ with aqueous solutions of Me(NO₃)₂.6H₂O and Pd(NO₃)₂H₂O. All samples were characterized by X-ray diffraction (XRD), temperature-programmed reduction (TPR), and X-ray photoelectron spectroscopy (XPS). An improvement of activity was observed after modification with different oxides. The results demonstrate that the Pd/Al₂O₃ catalysts modified with Co and Ce by impregnation with a common solution of respective salts, exhibit the most promising catalytic activity for methane oxidation. Most probably, the presence of Co₃O₄ and CeO₂ on catalytic surface increases surface oxygen and therefore leads to the better reactivity in methane combustion.

Keywords: methane combustion, palladium, Co-Ce, Ni-Ce

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Authors: Yekta Ülgen, Fırat Matur

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Cole-Cole parameters of 40 post-menopausal women are compared with their DEXA bone mineral density measurements. Impedance characteristics of four extremities are compared; left and right extremities are statistically same, but lower extremities are statistically different than upper ones due to their different fat content. The correlation of Cole-Cole impedance parameters to bone mineral density (BMD) is observed to be higher for a dominant arm. With the post menopausal population, ANOVA tests of the dominant arm characteristic frequency, as a predictor for DEXA classified osteopenic and osteoporotic population around the lumbar spine, is statistically very significant. When used for total lumbar spine osteoporosis diagnosis, the area under the Receiver Operating Curve of the characteristic frequency is 0.875, suggesting that the Cole-Cole plot characteristic frequency could be a useful diagnostic parameter when integrated into standard screening methods for osteoporosis. Moreover, the characteristic frequency can be directly measured by monitoring frequency driven the angular behavior of the dominant arm without performing any complex calculation.

Keywords: bioimpedance spectroscopy, bone mineral density, osteoporosis, characteristic frequency, receiver operating curve

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Authors: Hande Taşdemir, Meral Şahin, Mehmet Saçak

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Conductive composite materials obtained by physical or chemical mixing of two or more components having conducting and insulating properties have been increasingly attracted. Kaolinite in kaolin clays is one of silicates with two layers of molecular sheets of (Si2O5)2− and [Al2(OH)4]2+ with the chemical composition Al2Si2O5(OH)4. The most abundant hydrophillic kaolinite is extensively used in industrial processes and therefore it is convenient for the preparation of organic/inorganic composites. In this study, conductive poly(N-ethylaniline)/kaolinite composite was prepared by chemical polymerization of N-ethyl aniline in the presence of kaolinite particles using ammonium persulfate as oxidant in aqueous acidic medium. Poly(N-ethylaniline) content and conductivity of composite prepared were systematically investigated as a function of polymerization conditions such as ammonium persulfate, N-ethyl aniline and HCl concentrations. Poly(N-ethylaniline) content and conductivity of composite increased with increasing oxidant and monomer concentrations up to 0.1 M and 0.2 M, respectively, and decreased at higher concentrations. The maximum yield of polymer in the composite (15.0%) and the highest conductivity value of the composite (5.0×10-5 S/cm) was achieved by polymerization for 2 hours at 20°C in HCl of 0.5 M. The structure, morphological analyses and thermal behaviours of poly(N-ethylaniline)/kaolinite composite were characterized by FTIR and XRD spectroscopy, SEM and TGA techniques.

Keywords: kaolinite, poly(N-ethylaniline), conductive composite, chemical polymerization

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Authors: A. M. El-Aziz, M. Elsehamy, H. Hussein

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Steel or stainless steel have reasonable corrosion behavior in water, their corrosion resistance is significantly dependent on the water purity. It was not expected that demineralized water has an aggressive effect on steel alloys, in this study, the effect of water with different purity on steel X52 and stainless steel 316L was investigated. Weight loss and electrochemical measurements were employed to measure the corrosion behavior. Samples were microscopically investigated after test. It was observed that the higher the water purity the more reactive it is. Comparative analysis of the potentiodynamic curves for different water purity showed the aggressiveness of the demineralised water (conductivity of 0.05 microSiemens per cm) over the distilled water. Whereas, the corrosion rates of stainless steel 858 and 623 nm/y for demi and distilled water respectively. On the other hand, the corrosion rates of carbon steel x52 were estimated about 4.8 and 3.6 µm/y for demi and distilled water, respectively. Open circuit potential (OCP) recorded more positive potentials in case of stainless steel than carbon steel in different water purities. Generally, stainless steel illustrated high pitting resistance than carbon steel alloy, the surface film was investigated by scanning electron microscopy (SEM) and analyzed by energy dispersive X-ray spectroscopy (EDX). This behavior was explained based on that demi and distilled water might be considered as ‘hungry water’ in which it wants to be in equilibrium and will pull ions out of the surrounding metals trying to satisfy its ‘hunger’.

Keywords: corrosion, demineralized water, distilled water, steel alloys

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Authors: Nagasamy Venkatesh Dhandapani, Amged Awad El-Gied

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Cefixime, a BCS class II drug, is insoluble in water but freely soluble in acetone and in alcohol. The aqueous solubility of cefixime in water is poor and exhibits exceptionally slow and intrinsic dissolution rate. In the present study, cefixime and β-Cyclodextrin (β-CD) solid dispersions were prepared with a view to study the effect and influence of β-CD on the solubility and dissolution rate of this poorly aqueous soluble drug. Phase solubility profile revealed that the solubility of cefixime was increased in the presence of β-CD and was classified as A_L-type. Effect of variable, such as drug:carrier ratio, was studied. Physical characterization of the solid dispersion was characterized by Fourier transform infrared spectroscopy (FT-IR) and Differential scanning calorimetry (DSC). These studies revealed that a distinct loss of drug crystallinity in the solid molecular dispersions is ostensibly accounting for enhancement of dissolution rate in distilled water. The drug release from the prepared solid dispersion exhibited a first order kinetics. Solid dispersions of cefixime showed a 6.77 times fold increase in dissolution rate over the pure drug.

Keywords: β-cyclodextrin, cefixime, dissolution, Kneading method, solid dispersions, release kinetics

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Authors: H. Elmsellem, A. Aouniti, S. Radi, A. Chetouani, B. Hammouti

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The synthesis of new organic molecules offers various molecular structures containing heteroatoms and substituents for corrosion protection in acid pickling of metals. The most synthesized compounds are the nitrogen heterocyclic compounds, which are known to be excellent complex or chelate forming substances with metals. The choice of the inhibitor is based on two considerations: first it could be synthesized conveniently from relatively cheap raw materials, secondly, it contains the electron cloud on the aromatic ring or, the electro negative atoms such as nitrogen and oxygen in the relatively long chain compounds. In the present study, (NE)‐2‐methyl‐N‐(thiophen‐2‐ylmethylidene) aniline(T) was synthesized and its inhibiting action on the corrosion of mild steel in 1 M hydrochloric acid was examined by different corrosion methods, such as weight loss, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The experimental results suggest that this compound is an efficient corrosion inhibitor and the inhibition efficiency increases with the increase in inhibitor concentration. Adsorption of this compound on mild steel surface obeys Langmuir’s isotherm. Correlation between quantum chemical calculations and inhibition efficiency of the investigated compound is discussed using the Density Functional Theory method (DFT).

Keywords: mild steel, Schiff base, inhibition, corrosion, HCl, quantum chemical

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Authors: Nirmala Deenadayalu, Kwanele B. Mazibuko, Lethiwe D. Mthembu

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Sugarcane bagasse is the residue obtained after the extraction of sugar from the sugarcane. The main aim of this work was to produce catechol from sugarcane bagasse. The optimization of catechol production was investigated using a Box-Behnken design of experiments. The sugarcane bagasse was heated in a Parr reactor at a set temperature. The reactions were carried out at different temperatures (100-250) °C, catalyst loading (1% -10% KOH (m/v)) and reaction times (60 – 240 min) at 17 bar pressure. The solid and liquid fractions were then separated by vacuum filtration. The liquid fraction was analyzed for catechol using high-pressure liquid chromatography (HPLC) and characterized for the functional groups using Fourier transform infrared spectroscopy (FTIR). The optimized condition for catechol production was 175 oC, 240 min, and 10 % KOH with a catechol yield of 79.11 ppm. Since the maximum time was 240 min and 10 % KOH, a further series of experiments were conducted at 175 oC, 260 min, and 20 % KOH and yielded 2.46 ppm catechol, which was a large reduction in catechol produced. The HPLC peak for catechol was obtained at 2.5 min for the standards and the samples. The FTIR peak at 1750 cm⁻¹ was due to the C=C vibration band of the aromatic ring in the catechol present for both the standard and the samples. The peak at 3325 cm⁻¹ was due to the hydrogen-bonded phenolic OH vibration bands for the catechol. The ANOVA analysis was also performed on the set of experimental data to obtain the factors that most affected the amount of catechol produced.

Keywords: catechol, sugarcane bagasse, lignin, hydrothermal liquefaction

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Authors: V. Balamuralidhara

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The aim of the present work was to develop Paclitaxel loaded polyacrylamide grafted guar gum nanoparticles as pH responsive nanoparticle systems for targeting colon. The pH sensitive nanoparticles were prepared by modified ionotropic gelation technique. The prepared nanoparticles showed mean diameters in the range of 264±0.676 nm to 726±0.671nm, and a negative net charge 10.8 mV to 35.4mV. Fourier Transformed Infrared Spectroscopy (FT-IR) and Differential Scanning Calorimetry (DSC) studies suggested that there was no chemical interaction between drug and polymers. The encapsulation efficiency of the drug was found to be 40.92% to 48.14%. The suitability of the polyacrylamide grafted guar gum ERN’s for the release of Paclitaxel was studied by in vitro release at pH 1.2 and 7.4. It was observed that, there was no significant amount of drug release at gastric pH and 97.63% of drug release at pH 7.4 was obtained for optimized formulation F3 at the end of 12 hrs. In vivo drug targeting performance for the prepared optimized formulation (F3) and pure drug Paclitaxel was evaluated by HPLC. It was observed that the polyacrylamide grafted guar gum can be used to prepare nanoparticles for targeting the drug to the colon. The release performance was greatly affected by the materials used in ERN’s preparation, which allows maximum release at colon’s pH. It may be concluded that polyacrylamide grafted guar gum nanoparticles loaded with paclitaxel have desirable release responsive to specific pH. Hence it is a unique approach for colonic delivery of drug having appropriate site specificity and feasibility and controlled release of drug.

Keywords: colon targeting, polyacrylamide grafted guar gum nanoparticles, paclitaxel, nanoparticles

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Authors: Akash Bera, Suraj Singh, Jacinta Dsouza, Ramakrishna V. Hosur, Pushpa Mishra

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Ultraviolet C (UVC) radiation induces apoptosis in mammalian cells and it is suggested that the mechanism by which this occurs is the mitochondrial pathway of apoptosis through the release of cytochrome c from the mitochondria into the cytosol. The Bcl-2 family of proteins pro-and anti-apoptotic is the regulators of the mitochondrial pathway of apoptosis. Upon UVC irradiation, the proliferation of apoptosis is enhanced through the downregulation of the anti-apoptotic protein Bcl-xl and up-regulation of Bax. Although the participation of the Bcl-2 family of proteins in apoptosis appears responsive to UVC radiation, to the author's best knowledge, it is unknown how the structure and, effectively, the function of these proteins are directly impacted by UVC exposure. In this background, we present here a structural rationale for the effect of UVC irradiation in restoring apoptosis using two of the relevant proteins, namely, Bid-FL and Bcl-xl ΔC, whose solution structures have been reported previously. Using a variety of biophysical tools such as circular dichroism, fluorescence and NMR spectroscopy, we show that following UVC irradiation, the structures of Bcl-xlΔC and Bid-FL are irreversibly altered. Bcl-xLΔC is found to be more sensitive to UV exposure than Bid-FL. From the NMR data, dramatic structural perturbations (α-helix to β-sheet) are seen to occur in the BH3 binding region, a crucial segment of Bcl-xlΔC which impacts the efficacy of its interactions with pro-apoptotic tBid. These results explain the regulation of apoptosis by UVC irradiation. Our results on irradiation dosage dependence of the structural changes have therapeutic potential for the treatment of cancer.

Keywords: Bid, Bcl-xl, UVC, apoptosis

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Authors: Raul Guerrero, Sandro Machado, Miriam Carvalho

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Soil and aquifer pollution, caused by hydrocarbon liquid spilling, is induced by misguided operational practices and inefficient safety guidelines. According to the Environmental Brazilian Institute (IBAMA), during 2013 alone, over 472.13 m3 of diesel oil leaked into the environment nationwide for those reported cases only. Regarding the aforementioned information, there’s an indisputable need to adopt appropriate environmental safeguards specially in those areas intended for the production, treatment, transportation and storage of hydrocarbon fluids. According to Brazilian norm, ABNT-NBR 7505-1:2000, compacted soil or mineral barriers used in structural contingency levees, such as storage tanks, are required to present a maximum water permeability coefficient, k, of 1x10-6 cm/s. However, as discussed by several authors, water can not be adopted as the reference fluid to determine the site’s containment performance against organic fluids. Mainly, due to the great discrepancy observed in polarity values (dielectric constant) between water and most organic fluids. Previous studies, within this same research group, proposed an optimal range of values for the soil’s index properties for mineral barrier composition focused on organic fluid containment. Unfortunately, in some circumstances, it is not possible to encounter a type of soil with the required geotechnical characteristics near the containment site, increasing prevention and construction costs, as well as environmental risks. For these specific cases, the use of an organic product or material as an additive to enhance mineral-barrier containment performance may be an attractive geotechnical solution. This paper evaluates the effect of activated carbon (AC) content additions into a clayey soil towards hydrocarbon fluid permeability. Variables such as compaction energy, carbon texture and addition content (0%, 10% and 20%) were analyzed through laboratory falling-head permeability tests using distilled water and commercial diesel as percolating fluids. The obtained results showed that the AC with smaller particle-size reduced k values significantly against diesel, indicating a direct relationship between particle-size reduction (surface area increase) of the organic product and organic fluid containment.

Keywords: activated carbon, clayey soils, permeability, surface area

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Authors: Mohit Kalra, Varun S., Mayuri Gandhi

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

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

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Authors: Rosli Mohd Yunus, A. K. M. Moshiul Alam, Mohammad Dalour Beg

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In the case of advance polymeric materials reinforcement and thermal stability of matrix is a focused arena of researchers. The distribution of carbon nanotubes (CNTs) in polymer matrix influences material properties. In this study, multi-walled carbon nanotubes (MWCNTs) have been dispersed in unsaturated polyester resin (UPR) through solution mixing and sonication techniques using tetra hydro furan (THF) solvent. Nanocomposites have been fabricated with solution mixing and without solution mixing. Viscosity, Fourier-transform infrared spectroscopy, Field emission scanning electron microscopy (FESEM) investigations have been conducted to study the distribution as well as interaction between matrix and MWCNT. The differential scanning calorimetry (DSC), thermogravimetric analyses (TGA) and pyrolysis behavior have been conducted to study the thermal degradation and stability of nanocomposites. In addition, the SEM micrographs of nanocomposite residual chars were exhibited more packed together. Incorporation of CNT enhances crystallinity and mechanical and thermal properties of the nanocomposites. Correlations among MWCNTs dispersion, nucleation, fracture morphology and various properties have been made.

Keywords: char, multiwall carbon nanotubes, nano composite, pyrolysis

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Authors: Subodh N. Patel, Abhijit Pusty, Manashi Adhikary, Sandip Bhattacharyya

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The steam superheater (SH) is a coil type heat exchanger which is used to produce superheated steam or to convert the wet steam to dry steam (69.6 kg/cm² and 495°C), generated by a boiler. There were two superheaters in the system, SH I and SH II. SH II is a set of tubes that faces the initial interaction with flue gas at high temperature followed by SH I tubes. After a service life of 2100 hours, a tube in the SH II found to be punctured. Dye penetrant test revealed that out of 50 such tubes, 14 more tubes had severe cracks at a similar location. The failure was investigated in detail. The materials and scale were characterized by optical microscope and advance characterization technique. Scale, observed on fracture surface, was characterized under scanning electron microscope and Raman spectroscopy. Stresses acting on the tubes in working condition were analyzed by finite element method software, ANSYS. Cyclic stresses were observed in the simulation at the same prone location due to restriction in expansion of tubes. Based on scale characterization and stress analysis, it was concluded that the tube failed in thermo-mechanical fatigue. Finally, prevention and control measures were taken to avoid such failure in the future.

Keywords: finite element analysis, oxide scale, superheater tube, thermomechanical fatigue

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Authors: A. L. R. Rangel, J. A. M. Chaves, A. P. R. Alves Claro

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Surface modification of titanium and its alloys using TiO2 nanotube growth has been widely studied for biomedical field due to excellent interaction between implant and biological environment. The success of this treatment is directly related to anatase phase formation (TiO2 phase) which affects the cells growth. The aim of this study was to evaluate the phases formed in the nanotubes growth on the Ti-15Mo surface. Nanotubes were grown by electrochemical anodization of the alloy in ammonium fluoride based glycerol electrolyte for 24 hours at 20V. Then, the samples were annealed at 200°,400°, 450°, 500°, 600°, and 800° C for 1 hour. Contact angles measurements, scanning electron microscopy images and X rays diffraction analysis (XRD) were carried out for all samples. Raman Spectroscopy was used to evaluate TiO2 phases transformation in nanotubes samples as well. The results of XRD showed anatase formation for lower temperatures, while at 800 ° C the rutile phase was observed all over the surface. Raman spectra indicate that this phase transition occurs between 500 and 600 °C. The different phases formed have influenced the nanotubes morphologies, since higher annealing temperatures induced agglutination of the TiO2 layer, disrupting the tubular structure. On the other hand, the nanotubes drastically reduced the contact angle, regardless the annealing temperature.

Keywords: nanotubes, TiO2, titanium alloys, Ti-15Mo

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Authors: Madhurima Poddar, Vinay Sharma, Shaikh M. Mobin, Rajneesh Misra

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Three 1,8-naphthalimide (NPI) substituted 4,4-difluoroboradiaza-s-indacene (BODIPY) dyads were synthesized via Pd-catalyzed Sonogashira cross-coupling reaction of ethynyl substituted NPI with the meso-, β- and α-halogenated BODIPYs, respectively. The photophysical and electrochemical data reveals considerable electronic communication between the BODIPY and NPI moieties. The electronic absorption spectrum reveals that the substitution of NPI at α position of BODIPY exhibit better electronic communication between the NPI and the BODIPY units. The electronic structures of all the dyads exhibit planar geometries which are in a good correlation with the structures obtained from single crystal X-ray diffraction. The crystal structures of the dyads exhibit interesting supramolecular interactions. The dyads show good cytocompatibility with the potential of multicolor live-cell imaging; making them excellent candidates for biological applications. The work provides an important strategy of screening the substitution pattern at different position of BODIPYs which will be useful for the design of BODIPY based organic molecules for various optoelectronic applications as well as bio-imaging.

Keywords: bio-imaging studies, cross-coupling, cyclic voltammetry, density functional calculations, fluorescence spectra, single crystal XRD, UV/Vis spectroscopy

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Authors: P. Shrivastava, S. Vijayalakshmi, A. K. Singh, S. Dalai, R. Teotia, P. Sharma, J. Bellare

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This paper focuses on the synthesis and application of nanobioactive glass for bone regeneration studies. Nanobioactive glass has been synthesized by sol gel method having a combination of silicon, calcium and phosphorous in the molar ratio of 75:21:4. The prepared particles were analyzed for surface morphology by FEG SEM and FEG TEM. Physiochemical properties were investigated using ICP AES, FTIR spectroscopy and X-ray diffraction (XRD) techniques. To ascertain their use for therapeutic use, biocompatibility evaluation of the particles was done by performing soaking studies in SBF and in vitro cell culture studies on MG63 cell lines. Cell morphology was observed by FE SEM and phase contrast microscopy. Nanobioactive glasses (NBG) thus prepared were of 30-200 nm in size, which makes them suitable for nano-biomedical applications. The spherical shape of the particles imparts high surface to volume ratio, promoting fast growth of hydroxyapatite (HA), which is the mineral component of bone. As evaluated by in vitro cell culture studies the NBG was found to enhance the surface activation which enhances osteoblast adhesion. This is an essential parameter to improve bone tissue integration, thereby making nanobioactive glass therapeutically suitable for correcting bone defects.

Keywords: biocompatibility, bone tissue engineering, hydroxyapatite, nanobioactive glass

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Authors: Vusumzi E. Pakade, Themba D. Ntuli, Augustine E. Ofomaja

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Macadamia nutshell biosorbents treated in three different methods (raw Macadamia nutshell powder (RMN), acid-treated Macadamia nutshell (ATMN) and base-treated Macadamia nutshell (BTMN)) were investigated for the adsorption of Cr(VI) from aqueous solutions. Fourier transform infrared spectroscopy (FT-IR) spectra of free and Cr(VI)-loaded sorbents as well as thermogravimetric analysis (TGA) revealed that the acid and base treatments modified the surface properties of the sorbents. The optimum conditions for the adsorption of Cr(VI) by sorbents were pH 2, contact time 10 h, adsorbent dosage 0.2 g L-1, and concentration 100 mg L-1. The different treatment methods altered the surface characteristics of the sorbents and produced different maximum binding capacities of 42.5, 40.6 and 37.5 mg g-1 for RMN, ATMN and BTMN, respectively. The data was fitted into the Langmuir, Freundlich, Redlich-Peterson and Sips isotherms. No single model could clearly explain the data perhaps due to the complexity of process taking place. The kinetic modeling results showed that the process of Cr(VI) biosorption with Macadamia sorbents was better described by a process of chemical sorption in pseudo-second order. These results showed that the three treatment methods yielded different surface properties which then influenced adsorption of Cr(VI) differently.

Keywords: biosorption, chromium(VI), isotherms, Macadamia, reduction, treatment

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Authors: M. Bouhoun Ali, A. Y. Badjah Hadj Ahmed, M. Attou, A. Elias, M. A. Didi

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The extraction of uranium(VI) from aqueous solutions has been investigated using 1-hydroxyhexadecylidene-1,1-diphosphonic acid (HHDPA) and 1-hydroxydodecylidene-1,1-diphosphonic acid (HDDPA), which were synthesized and characterized by elemental analysis and by FT-IR, 1H NMR, 31P NMR spectroscopy. In this paper, we propose a tentative assignment for the shifts of those two ligands and their specific complexes with uranium(VI). We carried out the extraction of uranium(VI) by HHDPA and HDDPA from [carbon tetrachloride + 2-octanol (v/v: 90%/10%)] solutions. Various factors such as contact time, pH, organic/aqueous phase ratio and extractant concentration were considered. The optimum conditions obtained were: contact time= 20 min, organic/aqueous phase ratio = 1, pH value = 3.0 and extractant concentration = 0.3M. The extraction yields are more significant in the case of the HHDPA which is equipped with a hydrocarbon chain, longer than that of the HDDPA. Logarithmic plots of the uranium(VI) distribution ratio vs. pHeq and the extractant concentration showed that the ratio of extractant to extracted uranium(VI) (ligand/metal) is 2:1. The formula of the complex of uranium(VI) with the HHDPA and the DHDPA is UO2(H3L)2 (HHDPA and DHDPA are denoted as H4L). A spectroscopic analysis has showed that coordination of uranium(VI) takes place via oxygen atoms.

Keywords: liquid-liquid extraction, uranium(vi), 1-hydroxyalkylidene-1, 1-diphosphonic acids, hhdpa, hddpa, aqueous solution

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Authors: Shruti Sakarkar, Jega Jegatheesan, Srinivasan Madapusi

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Photocatalytic membranes have shown great potential for the removal of an organic and inorganic pollutant from wastewater as it combines the degradation and antibacterial properties from photocatalysis and physical separation by the membrane in a single unit. Incorporation of the semiconductor in membrane structure results in enhancing the performance and the properties of the membrane. In this study porous ultrafiltration polyvinylidene fluoride (PVDF) membranes with entrapped TiO₂ nanoparticle were prepared by phase inversion method and further used for the degradation of reactive orange 16 (RO16). Prepared photocatalytic membranes were characterized by the scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), contact angle, and atomic force microscope (AFM). The addition of TiO₂ nanopartparticles improves the strength and thermal stability of the membrane. In particular hydrophilicity and permeability increases with the increase of TiO₂ nanoparticles into the membrane. The photocatalytic membrane achieves 80-85% degrdation of RO16. The impact of different parameters such as pH, concentration of photocatalyst, dye concentration and effect of H₂O₂ were analysed. The best conditions for dye degradation were an initial dye concentration of 50 mg/L, with a membrane containing TiO₂ loading of 2wt%. It was observed that in the presence of H₂O₂, degradation increases with increasing H₂O₂ concentration and reached up to 95-98%. The high quality permeates obtained from the photocatalytic membrane can be reused.

Keywords: photocatalytic membrane, TiO₂, PVDF, nanoparticles

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Authors: Tomilola J. Ajayi, Moses Ollengo, Lukas le Roux, Michael N. Pillay, Richard J. Staples, Shannon M. Biros Werner E. van Zyl

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The formation, characterization, and dye-sensitized solar cell application of nickel(II), zinc(II) and cadmium(II) ferrocenyl dithiophosphonate complexes were investigated. The multidentate monoanionic ligand [S₂PFc(OH)]¯ (L1) was synthesized from the reaction between ferrocenyl Lawesson’s reagent, [FcP(=S)μ-S]₂ (FcLR), (Fc = ferrocenyl) and water. Ligand L1 could potentially coordinate to metal centers through the S, S’ and O donor atoms. The reaction between metal salt precursors and L1 produced a Ni(II) complex of the type [Ni{S₂P(Fc)(OH)}₂] (1) (molar ratio 1:2), a tetranickel (II) complex of the type [Ni₂{S₂OP(Fc)}₂]₂ (2) (molar ratio (1:1), as well as a Zn(II) complex [Zn{S₂P(Fc)(OH)}₂]₂ (3), and a Cd(II) complex [Cd{S₂P(Fc)(OH)}₂]₂ (4). Complexes 1-4 were characterized by 1H and 31P NMR and FT-IR, and complexes 1 and 2 were additionally analysed by X-Ray crystallography. After co-sensitization, the DSSCs were characterized using UV-Vis, cyclic voltammetry, electrochemical impedance spectroscopy, and photovoltaic measurements (I-V curves). Overall finding shows that co-sensitization of our compounds with ruthenium dye N719 resulted in a better overall solar conversion efficiency than only pure N719 dye under the same experimental conditions. In conclusion, we report the first examples of dye-sensitized solar cells (DSSCs) co-sensitized with ferrocenyl dithiophosphonate complexes.

Keywords: dithiophosphonate, dye sensitized solar cell, co-sensitization, solar efficiency

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Authors: A. Bortkiewcz, A. Dudarewicz, P. Małecki, M. Kłaczyński, T. Wszołek, Małgorzata Pawlaczyk-Łuszczyńska

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Low-frequency noise (LFN) has been recognized as a special environmental pollutant. It is usually considered a broadband noise with the dominant content of low frequencies from 10 Hz to 250 Hz. A growing body of data shows that LFN differs in nature from other environmental noises, which are at comparable levels but not dominated by low-frequency components. The primary and most frequent adverse effect of LFN exposure is annoyance. Moreover, some recent investigations showed that LFN at relatively low A-weighted sound pressure levels (40−45 dB) occurring in office-like areas could adversely affect the mental performance, especially of high-sensitive subjects. It is well documented that high-frequency noise disturbs various types of human functions; however, there is very little data on the impact of LFN on well-being and health, including the cardiovascular system. Heart rate variability (HRV) is a sensitive marker of autonomic regulation of the circulatory system. Walker and co-workers found that LFN has a significantly more negative impact on cardiovascular response than exposure to high-frequency noise and that changes in HRV parameters resulting from LFN exposure tend to persist over time. The negative reactions of the cardiovascular system in response to LFN generated by wind turbines (20-200 Hz) were confirmed by Chiu. The scientific aim of the study is to assess the relationship between the spectral-temporal characteristics of LFN and the activity of the autonomic nervous system, considering the subjective assessment of annoyance, sensitivity to this type of noise, and cognitive and general health status. The study will be conducted in 20 male students in a special, acoustically prepared, constantly supervised room. Each person will be tested 4 times (4 sessions), under conditions of non-exposure (sham) and exposure to noise of wind turbines recorded at a distance of 250 meters from the turbine with different frequencies and frequency ranges: acoustic band 20 Hz-20 kHz, infrasound band 5-20 Hz, acoustic band + infrasound band. The order of sessions of the experiment will be randomly selected. Each session will last 1 h. There will be a 2-3 days break between sessions to exclude the possibility of the earlier session influencing the results of the next one. Before the first exposure, a questionnaire will be conducted on noise sensitivity, general health status using the GHQ questionnaire, hearing organ status and sociodemographic data. Before each of the 4 exposures, subjects will complete a brief questionnaire on their mood and sleep quality the night before the test. After the test, the subjects will be asked about any discomfort and subjective symptoms during the exposure. Before the test begins, Holter ECG monitoring equipment will be installed. HRV will be analyzed from the ECG recordings, including time and frequency domain parameters. The tests will always be performed in the morning (9-12) to avoid the influence of diurnal rhythm on HRV results. Students will perform psychological tests 15 minutes before the end of the test (Vienna Test System).

Keywords: neurovegetative control, heart rate variability (HRV), cognitive processes, low frequency noise

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Authors: Rajesh Panda, Jimi Tjong, Sanjay K. Nayak, Mohini M. Sain

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The aim of this manuscript was to evaluate the effect of chemical treatment of sisal fibre on the mechanical and viscoelastic properties of bio based epoxy/fibre composites. The composite samples were manufactured through a vacuum infusion process by adding alkyl phenols from cashew nutshell liquid (CSNL). Changes in the chemical structure of the sisal fibres resulting from the treatments were analyzed by Fourier transform infrared spectroscopy (FTIR). Both alkali and silane treatments produced enhancements in the mechanical properties of sisal fibre bundles. The alkali treatment, when combined with the silane treatment, the mechanical properties of epoxy composites notably improved (13%) in comparison to untreated sisal fibre reinforced composites.This was attributed to an enhanced fibre/matrix interface. The incorporation of CSNL into the sisal/epoxy composite enhanced the fibre-matrix interfacial properties because of the addition of -OH groups to the epoxy matrix. The incorporation of sisal fibre imparts stiffness to the epoxy matrix.

Keywords: phenalkamine, sisal fiber, vacuum infusion, cashew nutshell liquid, cashew nutshell liquid (CSNL)

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Authors: Eko S. Kunarti, Akhmad Syoufian, Indriana Kartini, Agnes

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Fe₃O₄/SiO₂/TiO₂ nanoparticles have been synthesized and applied as a photocatalyst for the recovery of gold from the mixture of Au(III) and Cu(II) ions. The synthesis was started by the preparation of magnetite (Fe₃O₄) using coprecipitation and sonication methods, followed by SiO₂ coating on magnetite using sol-gel reactions, and then TiO₂ coating using sol-gel process. Characterization was performed by using infrared spectroscopy, X-ray diffraction, transmission electron microscopy methods. Activity of Fe₃O₄/SiO₂/TiO₂ nanoparticles was evaluated as a photocatalyst for recovery of gold through photoreduction of Au(III) ions in Au(III) and Cu(II) ions mixture with a ratio of 1:1, in a closed reactor equipped with UV lamp. The photoreduction yield was represented as a percentage (%) of reduced Au(III) which was calculated by substraction of initial Au(III) concentration by the unreduced one. The unreduced Au(III) was determined by atomic absorption spectrometry. Results showed that the Fe₃O₄/SiO₂/TiO₂ nanoparticles were successfully synthesised with excellent magnetic and photocatalytic properties. The nanoparticles present optimum activity at a pH of 5 under UV irradiation for 120 minutes. At the optimum condition, the Fe₃O₄/SiO₂/TiO₂ nanoparticles could reduce Au³⁺ to Au⁰ 97.24%. In the mixture of Au(III) and Cu(II) ions, the Au(III) ions are more easily reducible than Cu(II) ions with the reduction results of 96.9% and 45.80% for Au(III) and Cu(II) ions, respectively. In addition, the presence of Cu(II) ions has no significant effect on the amount of gold recovered and its reduction reaction rate.

Keywords: Fe₃O₄/SiO₂/TiO₂, photocatalyst, recovery, gold, Au(III) and Cu(II) mixture

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Authors: D. S. Fardhyanti, M. Megawati, H. Prasetiawan, U. Mediaty

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Currently, fossil fuel is supplying most of world’s energy resources. However, fossil fuel resources are depleted rapidly and require an alternative energy to overcome the increasing of energy demands. Bio-oil is one of a promising alternative renewable energy resources which is converted from biomass through pyrolysis or fast pyrolysis process. Bio-oil is a dark liquid fuel, has a smelling smoke and usually obtained from sugar cane, wood, coconut shell and any other biomass. Sugar cane content analysis showed that the content of oligosaccharide, hemicellulose, cellulose and lignin was 16.69%, 25.66%, 51.27% and 6.38% respectively. Sugar cane is a potential sources for bio-oil production shown by its high content of cellulose. In this study, production of bio-oil from sugar cane bagasse was investigated via fast pyrolysis reactor. Fast pyrolysis was carried out at 500 °C with a heating rate of 10 °C and 1 hour holding time at pyrolysis temperature. Physical properties and chemical composition of bio-oil were analyzed. The viscosity, density, calorific value and molecular weight of produced bio-oil was 3.12 cp, 2.78 g/cm3, 11,048.44 cals/g, and 222.67 respectively. The Bio-oil chemical composition was investigated using GC-MS. Percentage value of furfural, phenol, 3-methyl 1,2-cyclopentanedione, 5-methyl-3-methylene 5-hexen-2-one, 4-methyl phenol, 4-ethyl phenol, 1,2-benzenediol, and 2,6-dimethoxy phenol was 20.76%, 16.42%, 10.86%, 7.54%, 7.05%, 7.72%, 5.27% and 6.79% respectively.

Keywords: bio-oil, pyrolysis, bagasse, sugar cane, gas chromatography-mass spectroscopy

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Authors: Subrata Kar, Banani Kundu, Papiya Nandy, Ruma Basu, Sukhen Das

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Natural montmorilollite clay is a common ingredient in pharmaceutical products, both as excipients and active support; hence considered as suitable candidate for Drug Delivery System. In this work, cationic detergent CTAB is used to increase the interlayer spacing of Na+-Montmoriollite clay to intercalate curcumin and methotrexate. Methotrexate is a folic acid antagonist, anti-proliferative and immunosuppressive agent; while curcumin is a bioactive constituent of rhizomes of Curcuma longa, possessing remarkable chemo-preventive and anti-inflammatory properties. The resultant inorganic-organic hybrids are characterized by X-ray diffraction (XRD), Infrared spectroscopy (FTIR) and Thermo Gravimetric Analysis (TGA) to confirm successful intercalation of curcumin and Methotrexate within clay layers. Pharmaceutical investigation of the hybrids is explored by studying the drug loading (%), encapsulation efficiency and release kinetics. Finally in-vitro studies are performed using cancer cells to find the effect of released curcumin to improve the sensitivity of clay bound methotrexate to ameliorate cell death compared to their effectiveness when used without the inorganic aluminosilicate vehicle.

Keywords: montmorillonite, methotrexate, curcumin, loading efficiency, release kinetics, anticancer activity

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Authors: Dionisios Panagiotaras, Dimitrios Papoulis, Elias Stathatos

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Microfibrous palygorskite and tubular halloysite clay mineral combined with nanocrystalline TiO2 are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 450 °C. The synthesis is employing nonionic surfactant molecule as pore directing agent along with acetic acid-based sol-gel route without addition of water molecules. Drying and thermal treatment of composite films ensure elimination of organic material lead to the formation of TiO2 nanoparticles homogeneously distributed on the palygorskite or halloysite surfaces. Nanocomposite films without cracks of active anatase crystal phase on palygorskite and halloysite surfaces are characterized by microscopy techniques, UV-Vis spectroscopy, and porosimetry methods in order to examine their structural properties. The composite palygorskite-TiO2 and halloysite-TiO2 films with variable quantities of palygorskite and halloysite were tested as photocatalysts in the photo-oxidation of Basic Blue 41 azo dye in water. These nanocomposite films proved to be most promising photocatalysts and highly effective to dye’s decoloration in spite of small amount of palygorskite -TiO2 or halloysite- TiO2 catalyst immobilized onto glass substrates mainly due to the high surface area and uniform distribution of TiO2 on clay minerals avoiding aggregation.

Keywords: halloysite, palygorskite, photocatalysis, titanium dioxide

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Authors: Amir Peyman Soleymani, Jasna Jankovic

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The augmented demand of the clean and renewable energy has necessitated the fuel cell and battery industries to produce more efficient devices at the lower prices, which can be achieved through the improvement of the electrode. Microstructural characterization, as one of the main materials development tools, plays a pivotal role in the production of better clean energy devices. In this study, methods for characterization and studying of the defects and components distribution were performed on the polymer electrolyte membrane fuel cell (PEMFC) and Li-ion battery (LIB) electrodes in 2D and 3D. The particles distribution, porosity, mechanical defects, and component distribution were studied by Scanning Electron Microscope (SEM), SEM-Focused Ion Beam (SEM-FIB), and Scanning Transmission Electron Microscope equipped with Energy Dispersive Spectroscopy (STEM-EDS). The 3D results obtained from X-ray Computed Tomography (XCT) revealed the pathways for electron and ion conductivity and defects progression maps. Computer-aided methods (Avizo) were employed to simulate the properties and performance of the microstructure in the electrodes. The suggestions were provided to improve the performance of PEMFCs and LIBs by adjusting the microstructure and the distribution of the components in the electrodes.

Keywords: PEM fuel cells, Li-ion batteries, 2D and 3D imaging, materials characterizations

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Authors: Dolapop Sribudda, Ura Pancharoen

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The separation of Hg(II) from produced water by hollow fiber contactors (HFC) was investigation. This system included of two hollow fiber modules in the series connecting. The first module used for the extraction reaction and the second module for stripping reaction. Aliquat336 extractant was fed from the organic reservoirs into the shell side of the first hollow fiber module and continuous to the shell side of the second module. The organic liquid was continuously feed recirculate and back to the reservoirs. The feed solution was pumped into the lumen (tube side) of the first hollow fiber module. Simultaneously, the stripping solution was pumped in the same way in tube side of the second module. The feed and stripping solution was fed which had a counter current flow. Samples were kept in the outlet of feed and stripping solution for 1 hour and characterized concentration of Hg(II) by Inductively Couple Plasma Atomic Emission Spectroscopy (ICP-AES). Feed solution was produced water from natural gulf of Thailand. The extractant was Aliquat336 dissolved in kerosene diluent. Stripping solution used was nitric acid (HNO3) and thiourea (NH2CSNH2). The effect of carrier concentration and type of stripping solution were investigated. Results showed that the best condition were 10 % (v/v) Aliquat336 and 1.0 M NH2CSNH2. At the optimum condition, the extraction and stripping of Hg(II) were 98% and 44.2%, respectively.

Keywords: Hg(II), hollow fiber contactor, produced water, wastewater treatment

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Authors: Abhijith N. V., Abhijit Pattnayak, Deepak Kumar

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Nowadays, a group of alloys, namely high entropy alloys (HEA), because of their excellent properties. However, the fabrication of HEAs requires multistage techniques, especially mill-ing, sieving, compaction, sintering, inert media, etc. These processes are laborious, costly, time-oriented, and unsuitable for commercial application. This study adopted a single-stage process-based HVOF thermal spray to develop HEA coating on SS304L substrates. The wear behavior of the deposited HEA coating was explored under different milling time durations (5h, 10h, and 15h, respectively). The effect of feedstock preparation, microstructure, surface chemistry, and mechanical and metallurgical properties on wear resistance was also investigated. The microstructure and composition of both coating and feedstock were evaluated by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis. Finally, the phase distribution was correlated by X-ray diffraction (XRD ) analysis. The results showed that 15h milled powder coating indicated better tribological than the base substrate and 5h,10h milled powder coating. A chemically stable Body Centered Cubic (BCC) solid solution phase was generated within the 15h milled powder-coated system, which resulted in superior tribological properties.

Keywords: high entropy alloys coating, wear mechanism, HVOF coating, microstructure

Procedia PDF Downloads 77