Search results for: surface enhanced raman spectroscopy (SERS)

Authors: S. Melvin Samuel, Jayanta Bhattacharya

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In the present study, a graphene oxide/chitosan (GO-CS) composite material was prepared and used as an adsorbent for the removal of methylene blue (MB) from aqueous solution. The synthesized GO-CS adsorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopes (SEM), transmission electron microscopy (TEM), Raman spectroscopy and thermogravimetric analysis (TGA). The removal of MB was conducted in batch mode. The effect of parameters influencing the adsorption of MB such as pH of the solution, initial MB concentration, shaking speed, contact time and adsorbent dosage were studied. The results showed that the GO-CS composite material has high adsorption capacity of 196 mg/g of MB solution at pH 9.0. Further, the adsorption of MB on GO-CS followed pseudo second order kinetics and equilibrium adsorption data well fitted by the Langmuir isotherm model. The study suggests that the GO-CS is a favorable adsorbent for the removal of MB from aqueous solution.

Keywords: Methylene blue, Graphene oxide-chitosan, Isotherms, Kinetics.

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Authors: Debraj Gangopadhyay, Moumita Das, Ranjan K. Singh, Poonam Tandon

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Creatinine is a toxic chemical waste generated from muscle metabolism. Abnormally high levels of creatinine in the body fluid indicate possible malfunction or failure of the kidneys. This leads to a condition termed as creatinine induced nephrotoxicity. N-acetylcysteine is an antioxidant drug which is capable of preventing creatinine induced nephrotoxicity and is helpful to treat renal failure in its early stages. Taurine is another antioxidant drug which serves similar purpose. The kidneys have a natural power that whenever reactive oxygen species radicals increase in the human body, the kidneys make an antioxidant shell so that these radicals cannot harm the kidney function. Taurine plays a vital role in increasing the power of that shell such that the glomerular filtration rate can remain in its normal level. Thus taurine protects the kidneys against several diseases. However, taurine also has some negative effects on the body as its chloramine derivative is a weak oxidant by nature. N-acetylcysteine is capable of inhibiting the residual oxidative property of taurine chloramine. Therefore, N-acetylcysteine is given to a patient along with taurine and this combination is capable of suppressing the negative effect of taurine. Both N-acetylcysteine and taurine being affordable, safe, and widely available medicines, knowledge of the mechanism of their combined effect on creatinine, the favored route of administration, and the proper dose may be highly useful in their use for treating renal patients. Raman spectroscopy is a precise technique to observe minor structural changes taking place when two or more molecules interact. The possibility of formation of a complex between a drug molecule and an analyte molecule in solution can be explored by analyzing the changes in the Raman spectra. The formation of a stable complex of creatinine with N-acetylcysteinein vitroin aqueous solution has been observed with the help of Raman spectroscopic technique. From the Raman spectra of the mixtures of aqueous solutions of creatinine and N-acetylcysteinein different molar ratios, it is observed that the most stable complex is formed at 1:1 ratio of creatinine andN-acetylcysteine. Upon drying, the complex obtained is gel-like in appearance and reddish yellow in color. The complex is hygroscopic and has much better water solubility compared to creatinine. This highlights that N-acetylcysteineplays an effective role in reducing the toxic effect of creatinine by forming this water soluble complex which can be removed through urine. Since the drug taurine is also known to be useful in reducing nephrotoxicity caused by creatinine, the aqueous solution of taurine with those of creatinine and N-acetylcysteinewere mixed in different molar ratios and were investigated by Raman spectroscopic technique. It is understood that taurine itself does not undergo complexation with creatinine as no additional changes are observed in the Raman spectra of creatinine when it is mixed with taurine. However, when creatinine, N-acetylcysteine and taurine are mixed in aqueous solution in molar ratio 1:1:3, several changes occurring in the Raman spectra of creatinine suggest the diminishing toxic effect of creatinine in the presence ofantioxidant drugs N-acetylcysteine and taurine.

Keywords: creatinine, creatinine induced nephrotoxicity, N-acetylcysteine, taurine

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Authors: Ibrahim Abdelfattah, Adel Ismail, Ahmed Helal, Mohamed Faisal

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Advanced oxidation technologies are an environment friendly approach for the remediation of industrial wastewaters. Here, one pot synthesis of mesoporous In₂O₃-TiO₂ nanocomposites at different In₂O₃ contents (0-3 wt%) have been synthesized through a facile sol-gel method to evaluate their photocatalytic performance for the degradation of the imazapyr herbicide and phenol under visible light and UV illumination compared with commercially available either Degussa P-25 or UV-100 Hombikat. The prepared mesoporous In₂O₃-TiO₂ nanocomposites were characterized by TEM, STEM, XRD, Raman FT-IR, Raman spectra and diffuse reflectance UV-visible. The bandgap energy of the prepared photocatalysts was derived from the diffuse reflectance spectra. XRD Raman's spectra confirmed that highly crystalline anatase TiO₂ phase was formed. TEM images show TiO₂ particles are quite uniform with 10±2 nm sizes with mesoporous structure. The mesoporous TiO₂ exhibits large pore volumes of 0.267 cm³g⁻¹ and high surface areas of 178 m²g⁻¹, but they become reduced to 0.211 cm³g⁻¹ and 112 m²g⁻¹, respectively upon In₂O₃ incorporation, with tunable mesopore diameter in the range of 5 - 7 nm. The 0.5% In₂O₃-TiO₂ nanocomposite is considered to be the optimum photocatalyst which is able to degrade 90% of imazapyr herbicide and phenol along 180 min and 60 min respectively. The proposed mechanism of this system and the role of In₂O₃ are explained by details.

Keywords: In₂O₃-TiO₂ nanocomposites, sol-gel method, visible light illumination, UV illumination, herbicide and phenol wastewater, removal

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Authors: Samira Naghdi, Kyong Yop Rhee

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Transfer-free synthesis of graphene on dielectric substrates is highly desirable but remains challenging. Here, by using a thin sacrificial platinum layer as a catalyst, graphene was deposited on a silicon substrate through a simple and transfer-free synthesis method. During graphene growth, the platinum layer evaporated, resulting in direct deposition of graphene on the silicon substrate. In this work, different growth conditions of graphene were optimized. Raman spectra of the produced graphene indicated that the obtained graphene was bilayer. The sheet resistance obtained from four-point probe measurements demonstrated that the deposited graphene had high conductivity. Reflectance spectroscopy of graphene-coated silicon showed a decrease in reflectance across the wavelength range of 200-800 nm, indicating that the graphene coating on the silicon surface had antireflection capabilities.

Keywords: antireflection coating, chemical vapor deposition, graphene, the sheet resistance

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Authors: Leila Mosafa, Majid Moghadam, Mohammad Shahedi

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In this work, pectinase was immobilized on the surface of silica-coated magnetite nanoparticles via covalent attachment. The magnetite-immobilized enzyme was characterized by Fourier transform infrared spectroscopy, X-ray powder diffraction, scanning electron microscopy and vibrating sample magnetometry techniques. Response surface methodology using Minitab Software was applied for statistical designing of operating conditions in order to immobilize pectinase on magnetic nanoparticles. The optimal conditions were obtained at 30°C and pH 5.5 with 42.97 µl pectinase for 2 h. The immobilization yield was 50.6% at optimized conditions. Compared to the free pectinase, the immobilized pectinase was found to exhibit enhanced enzyme activity, better tolerance to the variation of pH and temperature, and improved storage stability. Both free and immobilized samples reduced the viscosity of apple juice from 1.12 to 0.88 and 0.92 mm2s-1, respectively, after 30 min at their optimum temperature. Furthermore, the immobilized enzyme could be reused six consecutive cycles and the efficiency loss in viscosity reduction was found to be only 8.16%.

Keywords: magnetite nanoparticles, pectinase enzyme, immobilization, juice clarification, enzyme activity

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Authors: M. Al Azri, M. Elzain, K. Bouziane, S. M. Chérif

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n-Type 6H-SiC(0001) substrates were implanted with three fluencies of Mn+ 5x1015 Mn/cm2 (Mn content: 0.7%), 1x1016 (~2 %), and 5x1016 cm–2 (7%) with implantation energy of 80 keV and substrate temperature of 365ºC. The samples were characterized using Rutherford Backscattering and Channeling Spectroscopy (RBS/C), High-Resolution X-Ray Diffraction technique (HRXRD), micro-Raman Spectroscopy (μRS), and Superconducting Quantum Interference Device (SQUID) techniques. The aim of our work is to investigate implantation induced defects with dose and to study any correlation between disorder-composition and magnetic properties. In addition, ab-initio calculations were used to investigate the structural and magnetic properties of Mn-doped 6H-SiC. Various configurations of Mn sites and vacancy types were considered. The calculations showed that a substitutional Mn atom at Si site possesses larger magnetic moment than Mn atom at C site. A model is introduced to explain the dependence of the magnetic structure on site occupation. The magnetic properties of ferromagnetically (FM) and antiferromagnetically (AFM) coupled pairs of Mn atoms with and without neighboring vacancies have also been explored.

Keywords: ab-initio calculations, diluted magnetic semiconductors, magnetic properties, silicon carbide

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Authors: Shalini Singh, Sanjay K. Srivastava, Govind, Mukhtar. A. Khan, P. K. Singh

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Nanotechnology is revolutionizing the development of biosensors. Nanomaterials and nanofabrication technologies are increasingly being used to design novel biosensors. Sensitivity and other attributes of biosensors can be improved by using nanomaterials with unique chemical, physical, and mechanical properties in their construction. Silicon is a promising biomaterial that is non-toxic and biodegradable and can be exploited in chemical and biological sensing. Present study demonstrated the streptavidin–biotin interaction on silicon surfaces with different topographies such as flat and nanostructured silicon (nanowires) surfaces. Silicon nanowires with wide range of surface to volume ratio were prepared by electrochemical etching of silicon wafer. The large specific surface of silicon nanowires can be chemically modified to link different molecular probes (DNA strands, enzymes, proteins and so on), which recognize the target analytes, in order to enhance the selectivity and specificity of the sensor device. The interaction of streptavidin with biotin was carried out on 3-aminopropyltriethoxysilane (APTS) functionalized silicon surfaces. Fourier Transform Infrared Spectroscopy (FTIR) and X-ray Photoelectron Spectroscopy (XPS) studies have been performed to characterize the surface characteristics to ensure the protein attachment. Silicon nanowires showed the enhance protein attachment, as compared to flat silicon surface due to its large surface area and good molecular penetration to its surface. The methodology developed herein could be generalized to a wide range of protein-ligand interactions, since it is relatively easy to conjugate biotin with diverse biomolecules such as antibodies, enzymes, peptides, and nucleotides.

Keywords: FTIR, silicon nanowires, streptavidin-biotin, XPS

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Authors: Samar Aoujia, Théo Guérineaub, Rayan Zaitera, Evelyne Fargina, Younès Messaddeqb, Thierry Cardinala

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Two barium gallo-germanate glass series were elaborated to investigate the effect of the yttrium introduction on the glass physicochemical properties and crystallization behavior. One to twenty mol% of YO3/2 were either added into the glass matrix or substituted for gallium oxide. The glass structure was studied by Raman spectroscopy, and the thermal, optical, thermo-mechanical and physical properties are examined. The introduction of yttrium ions in both glass series increases the glass transition temperature, crystallization temperature, softening temperature, coefficient of linear thermal expansion and density. Through differential scanning calorimetry and X-ray diffraction analyses, it was found that competition occurs between the gallo-germanate zeolite-type phase and the yttrium-containing phase. From 13 mol% of YO3/2, the yttrium introduction impedes the formation of surface crystallization in these glasses.

Keywords: photonic, heavy-metal oxide, glass, crystallization

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Authors: Wilson Handoko, Farshid Pahlevani, Isha Singla, Himanish Kumar, Veena Sahajwalla

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Aluminium bronze alloys are well known for their superior abrasion, tensile strength and non-magnetic properties, due to the co-presence of iron (Fe) and aluminium (Al) as alloying elements and have been commonly used in many industrial applications. However, continuous exposure to the marine environment will accelerate the risk of a tendency to Al bronze alloys parts failures. Although a higher level of corrosion resistance properties can be achieved by modifying its elemental composition, it will come at a price through the complex manufacturing process and increases the risk of reducing the ductility of Al bronze alloy. In this research, the use of ironmaking slag and waste plastic as the input source for surface modification of Al bronze alloy was implemented. Microstructural analysis conducted using polarised light microscopy and scanning electron microscopy (SEM) that is equipped with energy dispersive spectroscopy (EDS). An electrochemical corrosion test was carried out through Tafel polarisation method and calculation of protection efficiency against the base-material was determined. Results have indicated that uniform modified surface which is as the result of selective diffusion process, has enhanced corrosion resistance properties up to 12.67%. This approach has opened a new opportunity to access various industrial utilisations in commercial scale through minimising the dependency on natural resources by transforming waste sources into the protective coating in environmentally friendly and cost-effective ways.

Keywords: aluminium bronze, waste-based surface modification, tafel polarisation, corrosion resistance

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Authors: Abebe Taye

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The interest in enhancing the performance of all-solid-state batteries featuring lithium metal anodes as a potential alternative to traditional lithium-ion batteries has prompted exploration into new avenues. A promising strategy involves transforming lithium-ion batteries into hybrid configurations by integrating lithium-ion and lithium-metal solid-state components. This study is focused on achieving stable lithium deposition and advancing the electrochemical capabilities of solid-state lithium hybrid batteries with anodes by incorporating mesocarbon microbeads (MCMBs) blended with silver nanoparticles. To achieve this, mesocarbon microbeads (MCMBs) blended with silver nanoparticles are coated on stainless-steel current collectors. These samples undergo a battery of analyses employing diverse techniques. Surface morphology is studied through scanning electron microscopy (SEM). The electrochemical behavior of the coated samples is evaluated in both half-cell and full-cell setups utilizing an argyrodite-type sulfide electrolyte. The stability of MCMBs in the electrolyte is assessed using electrochemical impedance spectroscopy (EIS). Additional insights into the composition are gleaned through X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and energy-dispersive X-ray spectroscopy (EDS). At an ultra-low N/P ratio of 0.26, stability is upheld for over 100 charge/discharge cycles in half-cells. When applied in a full-cell configuration, the hybrid anode preserves 60.1% of its capacity after 80 cycles at 0.3 C under a low N/P ratio of 0.45. In sharp contrast, the capacity retention of the cell using untreated MCMBs declines to 20.2% after a mere 60 cycles. The introduction of mesocarbon microbeads (MCMBs) combined with silver nanoparticles into the hybrid anode of solid-state lithium batteries substantially elevates their stability and electrochemical performance. This approach ensures consistent lithium deposition and removal, mitigating dendrite growth and the accumulation of inactive lithium. The findings from this investigation hold significant value in elevating the reversibility and energy density of lithium-ion batteries, thereby making noteworthy contributions to the advancement of more efficient energy storage systems.

Keywords: MCMB, lithium metal, hybrid anode, silver nanoparticle, cycling stability

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Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are used as core components of nuclear reactors due to their high wear resistance, good corrosion properties, and good mechanical stability at high temperatures. The present work simulates the contact between the calandria tube and the liquid injection shutdown system (LISS) nozzle. The Calandria tube is the outer covering of the pressure tube. Water flows inside the pressure tube through fuel claddings which produces vibration in the pressure tube along with vibration in the calandria tube. Fretting wear takes place at the point of contact between the calandria tube and the LISS nozzle. Fretting tests were performed under different conditions, such as; varying fretting duration (i.e., 1 to 4 hours), varying frequency (i.e., 5 to 6.5 Hz), and varying amplitude (100 to 400 µm). The formation of the oxide layer was observed during the fretting wear test; as a result, the worn product. The worn surfaces were analyzed with scanning electron microscopy (SEM) to analyze the wear mechanism involved in the fretting test, and Energy dispersive x-ray spectroscopy (EDS) and Raman spectroscopy were used to confirm the presence of an oxide layer on the worn surface. The oxide layer becomes more uniform with fretting duration in case of water submerged condition as compared to dry contact condition. The oxide layer is deeply removed at high amplitude due to the change of wear mechanism from adhesion to abrasion, as confirmed by the presence of micro ploughing and micro cutting. Low amplitude fretting favors the formation of the tribo-oxide layer.

Keywords: tribo-oxide layer, wear, mechanically mixed layer, zircaloy

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Authors: Jan Luxa, Vlastimil Mazanek, Petr Malinsky, Alexander Romanenko, Mariapompea Cutroneo, Vladimir Havranek, Josef Novak, Eva Stepanovska, Anna Mackova, Zdenek Sofer

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Using accelerated energetic ions is an interesting method for the introduction of structural changes in various carbon-based materials. This way, the properties can be altered in two ways: a) the ions lead to the formation of conductive pathways in graphene oxide structures due to the elimination of oxygen functionalities and b) doping with selected ions to form metal nanoclusters, thus increasing the conductivity. In this work, energetic beams were employed in two ways to prepare capacitor structures in graphene oxide (GO), reduced graphene oxide (rGO) and polyimide (PI) on a micro-scale. The first method revolved around using ion beam writing with a focused ion beam, and the method involved ion implantation via a polymeric mask. To prepare the polymeric mask, a direct spin-coating of PMMA on top of the foils was used. Subsequently, proton beam writing and development in isopropyl alcohol were employed. Finally, the mask was removed using acetone solvent. All three materials were exposed to ion beams with an energy of 2.5-5 MeV and an ion fluence of 3.75x10¹⁴ cm-² (1800 nC.mm-²). Thus, prepared microstructures were thoroughly characterized by various analytical methods, including Scanning electron microscopy (SEM) with Energy-Dispersive X-ray spectroscopy (EDS), X-ray Photoelectron spectroscopy (XPS), micro-Raman spectroscopy, Rutherford Back-scattering Spectroscopy (RBS) and Elastic Recoil Detection Analysis (ERDA) spectroscopy. Finally, these materials were employed and tested as sensors for humidity using electrical conductivity measurements. The results clearly demonstrate that the type of ions, their energy and fluence all have a significant influence on the sensory properties of thus prepared sensors.

Keywords: graphene, graphene oxide, polyimide, ion implantation, sensors

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Authors: Chen-Fu Wang, Lin-Ya Kung

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

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

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Authors: Lila A. Alkhattaby, Norah A. Alsayegh, Mohammad S. Ansari, Mohammad O. Ansari

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In this work, we doped zinc oxide ZnO with potassium K we have synthesized using the sol-gel method. Structural properties were depicted by X-ray diffractometer (XRD) and energy distribution spectroscopy, X-ray diffraction studies confirm the nanosized of the particles and favored orientations along the (100), (002), (101), (102), (110), (103), (200), and (112) planes confirm the hexagonal wurtzite structure of ZnO NPs. The optical properties study using the UV-Vis spectroscopy. The band gap decreases from 4.05 eV to 3.88 eV, the lowest band gap at 10% doped concentration. The photoluminescence (PL) spectroscopy results show two main peaks, a sharp peak at ≈ 384 nm in the UV region and a broad peak around 479 nm in the visible region. The highest intensity of the band-edge luminescence was for 2% doped concentration because of the combined effect of the decreased probability of nonradiative recombination and has better crystallinity.

Keywords: K doped ZnO, photoluminescence spectroscopy, UV-Vis spectroscopy, x-ray spectroscopy

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Authors: Theo H. G. Moundzounga

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Arsenic and 2-chlorophenol are priority pollutants that pose serious health threats to humans and ecology. An electrochemical sensor, based on graphitic carbon nitride (g-C₃N₄) and carbon dots (CDs), was fabricated and used for the determination of arsenic and 2-chlorophenol. The g-C₃N₄/CDs nanocomposite was prepared via microwave irradiation heating method and was dropped-dried on the surface of the glassy carbon electrode (GCE). Transmission electron microscopy (TEM), X-ray diffraction (XRD), photoluminescence (PL), Fourier transform infrared spectroscopy (FTIR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) were used for the characterization of structure and morphology of the nanocomposite. Electrochemical characterization was done by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrochemical behaviors of arsenic and 2-chlorophenol on different electrodes (GCE, CDs/GCE, and g-C₃N₄/CDs/GCE) was investigated by differential pulse voltammetry (DPV). The results demonstrated that the g-C₃N₄/CDs/GCE significantly enhanced the oxidation peak current of both analytes. The analytes detection sensitivity was greatly improved, suggesting that this new modified electrode has great potential in the determination of trace level of arsenic and 2-chlorophenol. Experimental conditions which affect the electrochemical response of arsenic and 2-chlorophenol were studied, the oxidation peak currents displayed a good linear relationship to concentration for 2-chlorophenol (R²=0.948, n=5) and arsenic (R²=0.9524, n=5), with a linear range from 0.5 to 2.5μM for 2-CP and arsenic and a detection limit of 2.15μM and 0.39μM respectively. The modified electrode was used to determine arsenic and 2-chlorophenol in spiked tap and effluent water samples by the standard addition method, and the results were satisfying. According to the measurement, the new modified electrode is a good alternative as chemical sensor for determination of other phenols.

Keywords: electrochemistry, electrode, limit of detection, sensor

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Authors: Vedanki Khandenwal, Pawan Srivastava, Kartick Tarafder, Subhasis Ghosh

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We present here the experimental realization of controlled doping of graphene monolayers through charge transfer by trapping selected organic molecules between the graphene layer and underlying substrates. This charge transfer between graphene and trapped molecule leads to controlled n-type or p-type doping in monolayer graphene (MLG), depending on whether the trapped molecule acts as an electron donor or an electron acceptor. Doping controllability has been validated by a shift in corresponding Raman peak positions and a shift in Dirac points. In the transfer characteristics of field effect transistors, a significant shift of Dirac point towards positive or negative gate voltage region provides the signature of p-type or n-type doping of graphene, respectively, as a result of the charge transfer between graphene and the organic molecules trapped within it. In order to facilitate the charge transfer interaction, it is crucial for the trapped molecules to be situated in close proximity to the graphene surface, as demonstrated by findings in Raman and infrared spectroscopies. However, the mechanism responsible for this charge transfer interaction has remained unclear at the microscopic level. Generally, it is accepted that the dipole moment of adsorbed molecules plays a crucial role in determining the charge-transfer interaction between molecules and graphene. However, our findings clearly illustrate that the doping effect primarily depends on the reactivity of the constituent atoms in the adsorbed molecules rather than just their dipole moment. This has been illustrated by trapping various molecules at the graphene−substrate interface. Dopant molecules such as acetone (containing highly reactive oxygen atoms) promote adsorption across the entire graphene surface. In contrast, molecules with less reactive atoms, such as acetonitrile, tend to adsorb at the edges due to the presence of reactive dangling bonds. In the case of low-dipole moment molecules like toluene, there is a lack of substantial adsorption anywhere on the graphene surface. Observation of (i) the emergence of the Raman D peak exclusively at the edges for trapped molecules without reactive atoms and throughout the entire basal plane for those with reactive atoms, and (ii) variations in the density of attached molecules (with and without reactive atoms) to graphene with their respective dipole moments provides compelling evidence to support our claim. Additionally, these observations were supported by first principle density functional calculations.

Keywords: graphene, doping, charge transfer, liquid phase exfoliation

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Authors: Surya Prakash Gajagouni, Akram Alfantazi, Imad Barsoum

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Austenitic stainless steels are widely recognized for their exceptional corrosion resistance and mechanical properties, rendering them indispensable materials across various industries from construction to biomedical applications. However, in chloride and high temperature atmosphere it to further enhance their surface properties, anodization has emerged as a promising surface treatment technique. Anodization modifies the surface of stainless steels by creating a protective oxide layer, improving corrosion resistance and imparting additional functional characteristics. This paper explores the structural and corrosion characteristics of anodized austenitic stainless steels (AISI 304) using a two-step anodic technique. We utilized a perchloric acid-based electrolyte followed by an ammonium fluoride-based electrolyte. This sequential approach aimed to cultivate deeper and intricately self-ordered nanopore oxide arrays on a substrate made of 304 stainless steel. Electron Microscopic (SEM and TEM) images revealed nanoporous layered structures with increased length and crack development correlating with higher voltage and anodization time. Surface composition and chemical oxidation state of surface-treated SS were determined using X-ray photoelectron spectroscopy (XPS) techniques, revealing a surface layer rich in Ni and suppressed Cr, resulting in a thin film composed of Ni and Fe oxide compared to untreated SS. Electrochemical studies demonstrated enhanced corrosion resistance in a strong alkaline medium compared to untreated SS. Understanding the intricate relationship between the structural features of anodized stainless steels and their corrosion resistance is crucial for optimizing the performance of these materials in diverse applications. This study aims to contribute to the advancement of surface engineering strategies for enhancing the durability and functionality of austenitic stainless steels in aggressive environments.

Keywords: austenitic stainless steel, anodization, nanoporous oxides, marine corrosion

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Authors: Imen Harabi, Hanae Toura, Safa Jemai, Bernabe Mari Soucase

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A promising alternative to traditional Quantum Dots QD materials, which contain toxic heavy elements such as lead and cadmium, sheds light on indium phosphide quantum dots (InP QDs) Owing to improve the quantum yields of photoluminescence and other properties. InP, InP/ZnS core/shell and InP/ZnS/ZnS core/shell/shell Quantum Dots (QDs) were synthetized by the hot injection method. The optical and structural properties of the core InP QDs, InP/ZnS QDs, and InP/ZnS/ZnS QDs have being considered by several techniques such as X-ray diffraction, transmission electron microscopy, optical spectroscopy, and photoluminescence. The average diameter of InP, InP/ZnS, and InP/ZnS/ZnS Quantum Dots (QDs) was varying between 10 nm, 5.4 nm, and 4.10 nm. This experience revealed that the surface morphology of the Quantum Dots has a more regular spherical form with color variation of the QDs in solution. The emission peak of colloidal InP Quantum Dots was around 530 nm, while in InP/ZnS, the emission peak is displayed and located at 598 nm. whilst for InP/ZnS/ZnS is placed at 610 nm. Furthermore, an enhanced PL emission due to a passivation effect in the ZnS-covered InP QDs was obtained. Add the XRD information FWHM of the principal peak of InP QDs was 63 nm, while for InP/ZnS was 41 nm and InP/ZnS/ZnS was 33 nm. The effect of the Zinc stearate precursor concentration on the optical, structural, surface chemical of InP and InP/ZnS and InP/ZnS/ZnS QDs will be discussed.

Keywords: indium phosphide, quantum dot, nanoparticle, core-shell, multishell, luminescence

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Authors: Camilla G. Goncalves, Benedito Christ, Walter Miyakawa, Antonio J. Abdalla

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This work aims to investigate the properties and microstructure of diamond-like carbon film deposited by pulsed laser deposition by ablation of a graphite target in a vacuum chamber on a steel substrate. The equipment was mounted to provide one laser beam. The target of high purity graphite and the steel substrate were polished. The mechanical and tribological properties of the film were characterized using Raman spectroscopy, nanoindentation test, scratch test, roughness profile, tribometer, optical microscopy and SEM images. It was concluded that the pulsed laser deposition (PLD) technique associated with the low-pressure chamber and a graphite target provides a good fraction of sp3 bonding, that the process variable as surface polishing and laser parameter have great influence in tribological properties and in adherence tests performance. The optical microscopy images are efficient to identify the metallurgical bond.

Keywords: characterization, DLC, mechanical properties, pulsed laser deposition

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Authors: Lucija Pustahija, Christine Bandl, Wolfgang Kern, Christian Mitterer

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Concerning today´s ecological demands, producing reliable materials from sustainable resources is a continuously developing topic. Such an example is the production of carbon materials via pyrolysis of natural gases or biomass. The amazing properties of pyrolytic carbon are utilized in various fields, where in particular the application in building industry is a promising way towards the utilization of pyrolytic carbon and composites based on pyrolytic carbon. For many applications, surface modification of carbon is an important step in tailoring its properties. Therefore, in this paper, an investigation of different oxidation methods was performed to prepare the carbon surface before functionalizing it with organosilanes, which act as coupling agents for epoxy and polyurethane resins. Made in such a way, a building material based on carbon composites could be used as a lightweight, durable material that can be applied where water or air filtration / purification is needed. In this work, both wet and dry oxidation were investigated. Wet oxidation was first performed in solutions of nitric acid (at 120 °C and 150 °C) followed by oxidation in hydrogen peroxide (80 °C) for 3 and 6 h. Moreover, a hydrothermal method (under oxygen gas) in autoclaves was investigated. Dry oxidation was performed under plasma and corona discharges, using different power values to elaborate optimum conditions. Selected samples were then (in preliminary experiments) subjected to a silanization of the surface with amino and glycidoxy organosilanes. The functionalized surfaces were examined by X-ray photon spectroscopy and Fourier transform infrared spectroscopy spectroscopy, and by scanning electron microscopy. The results of wet and dry oxidation methods indicated that the creation of functionalities was influenced by temperature, the concentration of the reagents (and gases) and the duration of the treatment. Sequential oxidation in aq. HNO₃ and H₂O₂ results in a higher content of oxygen functionalities at lower concentrations of oxidizing agents, when compared to oxidizing the carbon with concentrated nitric acid. Plasma oxidation results in non-permanent functionalization on the carbon surface, by which it´s necessary to find adequate parameters of oxidation treatments that could enable longer stability of functionalities. Results of the functionalization of the carbon surfaces with organosilanes will be presented as well.

Keywords: building materials, dry oxidation, organosilanes, pyrolytic carbon, resins, surface functionalization, wet oxidation

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Authors: Mingmei Zhang, Xinyong Li

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AgInS₂/SnS₂ (AIS) nanocomposites were synthesized by a simple hydrothermal method. The morphology and composition of the fabricated AIS nanocomposites were investigated by field-emission scanning electron microscopy (SEM), X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). Moreover, the as-prepared AIS photocatalysts exhibited excellent photocatalytic activities for the degradation of Norfloxacin (NOR), mainly due to its high optical absorption and separation efficiency of photogenerated electron-hole pairs, as evidenced by UV–vis diffusion reflection spectra (DRS) and Surface photovoltage (SPV) spectra. Furthermore, the interfacial charges transfer mechanism was also discussed by DFT calculations.

Keywords: AIS nanocomposites, electron-hole pairs, charges transfer, DFTcaculations

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Authors: Sami Iqbal, Azam Hussain, Weiping Wu, Guo Xinli, Tong Zhang

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A novel octagonal upright micro-pyramid structure was generated by wet chemical anisotropic etching on a monocrystalline silicon wafer (100). The primary objectives are to reduce front surface reflectance of silicon wafers, improve wettability, enhance surface morphology, and maximize the area coverage by generated octagonal pyramids. Under rigorous control and observation, the etching process' response time was maintained precisely. The experimental outcomes show a significant decrease in the optical surface reflectance of silicon wafers, with the lowest reflectance of 8.98%, as well as enhanced surface structure, periodicity, and surface area coverage of more than 85%. The octagonal silicon pyramid was formed with a high etch rate of 0.41 um/min and a much shorter reaction time with the addition of hydrofluoric acid coupled with magnetic stirring (mechanical agitation) at 300 rpm.

Keywords: octagonal pyramids, rapid etching, solar cells, surface engineering, surface reflectance

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Authors: Ariadne C. Catto, Luis F. da Silva, Khalifa Aguir, Valmor Roberto Mastelaro

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Zinc oxide (ZnO) pure or doped are one of the most promising metal oxide semiconductors for gas sensing applications due to the well-known high surface-to-volume area and surface conductivity. It was shown that ZnO is an excellent gas-sensing material for different gases such as CO, O2, NO2 and ethanol. In this context, pure and doped ZnO exhibiting different morphologies and a high surface/volume ratio can be a good option regarding the limitations of the current commercial sensors. Different studies showed that the sensitivity of metal-doped ZnO (e.g. Co, Fe, Mn,) enhanced its gas sensing properties. Motivated by these considerations, the aim of this study consisted on the investigation of the role of Co ions on structural, morphological and the gas sensing properties of nanostructured ZnO samples. ZnO and Zn1-xCoxO (0 < x < 5 wt%) thin films were obtained via the polymeric precursor method. The sensitivity, selectivity, response time and long-term stability gas sensing properties were investigated when the sample was exposed to a different concentration range of ozone (O3) at different working temperatures. The gas sensing property was probed by electrical resistance measurements. The long and short-range order structure around Zn and Co atoms were investigated by X-ray diffraction and X-ray absorption spectroscopy. X-ray photoelectron spectroscopy measurement was performed in order to identify the elements present on the film surface as well as to determine the sample composition. Microstructural characteristics of the films were analyzed by a field-emission scanning electron microscope (FE-SEM). Zn1-xCoxO XRD patterns were indexed to the wurtzite ZnO structure and any second phase was observed even at a higher cobalt content. Co-K edge XANES spectra revealed the predominance of Co2+ ions. XPS characterization revealed that Co-doped ZnO samples possessed a higher percentage of oxygen vacancies than the ZnO samples, which also contributed to their excellent gas sensing performance. Gas sensor measurements pointed out that ZnO and Co-doped ZnO samples exhibit a good gas sensing performance concerning the reproducibility and a fast response time (around 10 s). Furthermore, the Co addition contributed to reduce the working temperature for ozone detection and improve the selective sensing properties.

Keywords: cobalt-doped ZnO, nanostructured, ozone gas sensor, polymeric precursor method

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Authors: Surabhi Pandey, Pavuluri Srinivasa Rao

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Extrusion processing is a high-temperature short time (HTST) treatment which can improve protein quality and digestibility together with retaining active nutrients. In-vitro protein digestibility of plant protein-based foods is generally enhanced by extrusion. The current study aimed to investigate the effect of extrusion cooking on in-vitro protein digestibility (IVPD) and conformational modification of protein in green banana flour extrudates. Green banana flour was extruded through a co-rotating twin-screw extruder varying the moisture content, barrel temperature, screw speed in the range of 10-20 %, 60-80 °C, 200-300 rpm, respectively, at constant feed rate. Response surface methodology was used to optimise the result for IVPD. Fourier-transform infrared spectroscopy (FTIR) analysis provided a convenient and powerful means to monitor interactions and changes in functional and conformational properties of extrudates. Results showed that protein digestibility was highest in extrudate produced at 80°C, 250 rpm and 15% feed moisture. FTIR analysis was done for the optimised sample having highest IVPD. FTIR analysis showed that there were no changes in primary structure of protein while the secondary protein structure changed. In order to explain this behaviour, infrared spectroscopy analysis was carried out, mainly in the amide I and II regions. Moreover, curve fitting analysis showed the conformational changes produced in the flour due to protein denaturation. The quantitative analysis of the changes in the amide I and II regions provided information about the modifications produced in banana flour extrudates.

Keywords: extrusion, FTIR, protein conformation, raw banana flour, SDS-PAGE method

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Authors: Sara Mercedes Barroso Pinzón, Antonio Javier Sanchéz Herencia, Begoña Ferrari, Álvaro Jesús Castro

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The current need for durable implants and bone substitutes characterised by biocompatibility, bioactivity and mechanical properties, without immunological rejection, is a major challenge for scientists. Hydroxyapatite (HAp) has been considered for decades as an ideal biomaterial for bone regeneration due to its chemical and crystallographic similarity to the mineral structure bioapatites. However, the lack of trace elements in the hydroxyapatite structure gives it very low mechanical and biological properties. In this sense, the objective of the research is to address the synthesis of hydroxyapatite with Mg from phosphate rock from sedimentary deposits in the central-eastern region of Colombia, taking advantage of the release of the species contained as natural precursors of Ca, P and Mg. The minerals present were studied, fluorapatite as the mineral of interest associated with mineralogical species of magnesium carbonates and quartz. The chemical and mineralogical composition was determined by X-ray fluorescence (XRF) and X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX); as well as the evaluation of the surface physicochemical properties of zeta potential (PZC), with the aim of studying the surface behaviour of the microconstituents present in the phosphate rock and to elucidate the synergistic mechanism between the minerals and establish the optimum conditions for the wet concentration process. From the products obtained and characterised by XRD, XRF, SEM, FTIR, RAMAN, HAp-Mg biocomposite scaffolds are fabricated and the influence of Mg on the morphometric parameters, mechanical and biological properties of the designed materials is evaluated.

Keywords: phosphate rock, hydroxyapatite, magnesium, biomaterials

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Authors: I. Wlasny, Z. Klusek, A. Wysmolek

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Hexagonal boron nitride is a representative of a widely popular class of two-dimensional Van Der Waals materials. It finds its uses, among others, in construction of complexly layered heterostructures. Hexagonal boron nitride attracts great interest because of its properties characteristic for wide-gap semiconductors as well as an ultra-flat surface.Van Der Waals heterostructures composed of two-dimensional layered materials, such as transition metal dichalcogenides or graphene give hope for miniaturization of various electronic and optoelectronic elements. In our presentation, we will show the results of our investigations of the not previously reported modification of the hexagonal boron nitride layers with focused laser beam. The electrostatic force microscopy (EFM) images reveal that the irradiation leads to changes of the local electric fields for a wide range of laser wavelengths (from 442 to 785 nm). These changes are also accompanied by alterations of crystallographic structure of the material, as reflected by Raman spectra. They exhibit high stability and remain visible after at least five months. This behavior can be explained in terms of photoionization of the defect centers in h-BN which influence non-uniform electrostatic field screening by the photo-excited charge carriers. Analyzed changes influence local defect structure, and thus the interatomic distances within the lattice. These effects can be amplified by the piezoelectric character of hexagonal boron nitride, similar to that found in nitrides (e.g., GaN, AlN). Our results shed new light on the optical properties of the hexagonal boron nitride, in particular, those associated with electron-phonon coupling. Our study also opens new possibilities for h-BN applications in layered heterostructures where electrostatic fields can be used in tailoring of the local properties of the structures for use in micro- and nanoelectronics or field-controlled memory storage. This work is supported by National Science Centre project granted on the basis of the decision number DEC-2015/16/S/ST3/00451.

Keywords: atomic force microscopy, hexagonal boron nitride, optical properties, raman spectroscopy

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Authors: Yasemin Seki, Aysun Akşit

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The goal of this research is to modify the surface characterization of jute yarns with different chemical agents to improve the compatibility with a non-polar polymer, polypropylene, when used as reinforcement. A literature review provided no knowledge on surface treatment of jute fibers with sodium perborate trihydrate. This study also aims to compare the efficiency of sodium perborate trihydrate on jute fiber treatment with other commonly used chemical agents. Accordingly, jute yarns were treated with 0.02% potassium dichromate (PD), potassium permanganate (PM) and sodium perborate trihydrate (SP) aqueous solutions in order to enhance interfacial compatibility with polypropylene in this study. The effect of treatments on surface topography, surface chemistry and interfacial shear strength of jute yarns with polypropylene were investigated. XPS results revealed that surface treatments enhanced surface hydrophobicity by increasing C/O ratios of fiber surface. Surface roughness values increased with the treatments. The highest interfacial adhesion with polypropylene was achieved after SP treatment by providing the highest surface roughness values and hydrophobic character of jute fiber.

Keywords: jute, chemical modification, sodium perborate, polypropylene

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Authors: Makhan Maharjan, Mani Ulaganathan, Vanchiappan Aravindan, Srinivasan Madhavi, Jing-Yuan Wang, Tuti Mariana Lim

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The ever-increasing energy demand has made research to develop high performance energy storage systems that are able to fulfill energy needs. Supercapacitors have potential applications as portable energy storage devices. In recent years, there have been huge research interests to enhance the performances of supercapacitors via exploiting novel promising carbon precursors, tailoring textural properties of carbons, exploiting various electrolytes and device types. In this work, we employed orange peel (waste material) as the starting material and synthesized activated carbon by pyrolysis of KOH impregnated orange peel char at 800 °C in argon atmosphere. The resultant orange peel-derived activated carbon (OP-AC) exhibited BET surface area of 1,901 m² g-1, which is the highest surface area so far reported for the orange peel. The pore size distribution (PSD) curve exhibits the pores centered at 11.26 Å pore width, suggesting dominant microporosity. The high surface area OP-AC accommodates more ions in the electrodes and its well-developed porous structure facilitates fast diffusion of ions which subsequently enhance electrochemical performance. The OP-AC was studied as positive electrode in combination with different negative electrode materials, such as pre-lithiated graphite (LiC6) and Li4Ti5O12 for making hybrid capacitors. The lithium ion capacitor (LIC) fabricated using OP-AC with pre-lithiated graphite delivered high energy density of ~106 Wh kg–1. The energy density for OP-AC||Li4Ti5O12 capacitor was ~35 Wh kg⁻¹. For comparison purpose, configuration of OP-AC||OP-AC capacitors were studied in both aqueous (1M H2SO4) and organic (1M LiPF6 in EC-DMC) electrolytes, which delivered the energy density of 8.0 Wh kg⁻¹ and 16.3 Wh kg⁻¹, respectively. The cycling retentions obtained at current density of 1 A g⁻¹ were ~85.8, ~87.0 ~82.2 and ~58.8% after 2500 cycles for OP-AC||OP-AC (aqueous), OP-AC||OP-AC (organic), OP-AC||Li4Ti5O12 and OP-AC||LiC6 configurations, respectively. In addition, characterization studies were performed by elemental and proximate composition, thermogravimetry analysis, field emission-scanning electron microscopy, Raman spectra, X-ray diffraction (XRD) pattern, Fourier transform-infrared, X-ray photoelectron spectroscopy (XPS) and N2 sorption isotherms. The morphological features from FE-SEM exhibited well-developed porous structures. Two typical broad peaks observed in the XRD framework of the synthesized carbon implies amorphous graphitic structure. The ratio of 0.86 for ID/IG in Raman spectra infers high degree of graphitization in the sample. The band spectra of C 1s in XPS display the well resolved peaks related to carbon atoms in various chemical environments. The presence of functional groups is also corroborated from the FTIR spectroscopy. Characterization studies revealed the synthesized carbon to be promising electrode material towards the application for energy storage devices. Overall, the intriguing properties of OP-AC make it a new alternative promising electrode material for the development of high energy lithium ion capacitors from abundant, low-cost, renewable biomass waste. The authors gratefully acknowledge Agency for Science, Technology and Research (A*STAR)/ Singapore International Graduate Award (SINGA) and Nanyang Technological University (NTU), Singapore for funding support.

Keywords: energy storage, lithium-ion capacitors, orange peels, porous activated carbon

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Authors: Satam Alotibi, Haya A. Al-Sunaidi, Almaymunah M. AlRoibah, Zahraa H. Al-Omaran, Mohammed Alyami, Fatehia S. Alhakami, Abdellah Kaiba, Mazen Alshaaer, Talal F. Qahtan

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This research study presents a novel approach to harnessing the potential of natural geopolymer in conjunction with TiO₂ nanoparticles (TiO₂ NPs) for the development of highly efficient photocatalytic materials for water decontamination. The study begins with the formulation of a geopolymer paste derived from natural sources, which is subsequently applied as a coating on glass substrates and allowed to air-dry at room temperature. The result is a series of geopolymer-coated glass films, serving as the foundation for further experimentation. To enhance the photocatalytic capabilities of these films, a critical step involves immersing them in a suspension of TiO₂ nanoparticles (TiO₂ NPs) in water for varying durations. This immersion process yields geopolymer-loaded TiO₂ NPs films with varying concentrations, setting the stage for comprehensive characterization and analysis. A range of advanced analytical techniques, including UV-Vis spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM), were meticulously employed to assess the structural, morphological, and chemical properties of the geopolymer-based TiO₂ films. These analyses provided invaluable insights into the materials' composition and surface characteristics. The culmination of this research effort sees the geopolymer-based TiO₂ films being repurposed as immobilized photocatalytic reactors for water decontamination under natural sunlight irradiation. Remarkably, the results revealed exceptional photocatalytic performance that exceeded the capabilities of conventional TiO₂-based photocatalysts. This breakthrough underscores the significant potential of natural geopolymer as a versatile and highly effective matrix for enhancing the photocatalytic efficiency of TiO₂ nanoparticles in water treatment applications. In summary, this study represents a significant advancement in the quest for sustainable and efficient photocatalytic materials for environmental remediation. By harnessing the synergistic effects of natural geopolymer and TiO₂ nanoparticles, these geopolymer-based films exhibit outstanding promise in addressing water decontamination challenges and contribute to the development of eco-friendly solutions for a cleaner and healthier environment.

Keywords: geopolymer, TiO2 nanoparticles, photocatalytic materials, water decontamination, sustainable remediation

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Authors: Nadia Hammouda, Kamel Belmokre

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Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, seawater

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