Search results for: surface treated graphene

Authors: A. A. Salisu, M. Y. Yakasai, K. M. Aujara

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Sisal leaves were subjected to enzymatic retting method to extract the sisal fibre. A portion of the fibre was pretreated with alkali (NaOH), and further treated with benzoyl chloride and silane treatment reagents. Both the treated and untreated Sisal fibre composites were used to fabricate the composite by hand lay-up technique using unsaturated polyester resin. Tensile, flexural, water absorption, density, thickness swelling and chemical resistant tests were conducted and evaluated on the composites. Results obtained for all the parameters showed an increase in the treated fibre compared to untreated fibre. FT-IR spectra results ascertained the inclusion of benzoyl and silane groups on the fibre surface. Scanning electron microscopy (SEM) result obtained showed variation in the morphology of the treated and untreated fibre. Chemical modification was found to improve adhesion of the fibre to the matrix, as well as physico-mechanical properties of the composites.

Keywords: chemical resistance, density test, polymer matrix sisal fibre, thickness swelling

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Authors: Nikhil John Kollannur, Dali Naidu Arnepalli

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Most of the surface related phenomena in the case of fine-grained soil are attributed to their unique surface charge properties and specific surface area. The temporal variations in soil behavior, to some extent, can be credited to the changes in these properties. Among the multitude of factors that affect the charge and surface area of clay minerals, the inherent system chemistry occupies the cardinal position. The impact is more profound when the chemistry change is manifested in terms of the system pH. pH plays a significant role by modifying the edge charges of clay minerals and facilitating mineral dissolution. Hence there is a need to address the variations in physical and charge properties of fine-grained soils treated over a range of acidic as well as alkaline conditions. In the present study, three soils (two soils commercially procured and one natural soil) exhibiting distinct mineralogical compositions are subjected to different pH environment over a range of 2 to 13. The soil-solutions prepared at a definite liquid to solid ratio are adjusted to the required pH value by adding measured quantities of 0.1M HCl/0.1M NaOH. The studies are conducted over a range of interaction time, varying from 1 to 96 hours. The treated soils are then analyzed for their physical properties in terms of specific surface area and particle size characteristics. Further, modifications in surface morphology are evaluated from scanning electron microscope (SEM) imaging. Changes in the surface charge properties are assessed in terms of zeta potential measurements. Studies show significant variations in total surface area, probably because of the dissolution of clay minerals. This observation is further substantiated by the morphological analysis with SEM imaging. The zeta potential measurements on soils indicate noticeable variation upon pH treatment, which is partially ascribed to the modifications in the pH-dependant edge charges and partially due to the clay mineral dissolution. The results provide valuable insight into the role of pH in a clay-electrolyte system upon surface related phenomena such as species adsorption, fabric modification etc.

Keywords: acid and alkali treatment, mineral dissolution , specific surface area, zeta potential

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Authors: Johana Jaramillo, Robin Kalfat, Dmitriy A. Dikin

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The cement production process is one of the major sources of carbon dioxide (CO₂), a potent greenhouse gas. Indeed, as a result of its cement manufacturing process, concrete contributes approximately 8% of global greenhouse gas emissions. In addition to environmental concerns, concrete also has a low tensile and ductility strength, which can lead to cracks. Graphene nanoplatelets (GNPs) have proven to be an eco-friendly solution for improving the mechanical and durability properties of concrete. The current research investigates the effects of preparing concrete enhanced with GNPs by using different wet dispersions techniques and mixing methods on its mechanical properties. Concrete specimens were prepared with 0.00 wt%, 0.10 wt%, 0.20 wt%, 0.30 wt% and wt% GNPs. Compressive and flexural strength of concrete at age 7 days were determined. The results showed that the maximum improvement in mechanical properties was observed when GNPs content was 0.20 wt%. The compressive and flexural were improved by up to 17.5% and 8.6%, respectively. When GNP dispersions were prepared by the combination of a drill and an ultrasonic probe, mechanical properties experienced maximum improvement.

Keywords: concrete, dispersion techniques, graphene nanoplatelets, mechanical properties, mixing methods

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Authors: Kumar N., Verma S., Park J., Srivastava V. C.

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Organic carbonates have the potential to be used as fuels and because of this, their production through non-phosgene routes is a thrust area of research. Di-ethyl carbonate (DEC) synthesis from propylene carbonate (PC) in the presence of alcohol is a green route. In this study, the use of reduced graphene oxide (rGO) based metal oxide catalysts [rGO-MO, where M = Ce] with different amounts of graphene oxide (0.2%, 0.5%, 1%, and 2%) has been investigated for the synthesis of DEC by using PC and ethanol as reactants. The GO sheets were synthesized by an electrochemical process and the catalysts were synthesized using an in-situ method. A theoretical study of the thermodynamics of the reaction was done, which revealed that the reaction is mildly endothermic. The theoretical value of optimum temperature was found to be 420 K. The synthesized catalysts were characterized for their morphological, structural and textural properties using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), N2 adsorption/desorption, thermogravimetric analysis (TGA), and Raman spectroscopy. Optimization studies were carried out to study the effect of different reaction conditions like temperature (140 °C to 180 °C) and catalyst dosage (0.102 g to 0.255 g) on the yield of DEC. Amongst the various synthesized catalysts, 1% rGO-CeO2 gave the maximum yield of DEC.

Keywords: GO, DEC, propylene carbonate, transesterification, thermodynamics

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Authors: Iftikhar Ahmad, Mohammad Islam

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Thermally exfoliated graphene nanomaterial was reinforced into Al2O3 ceramic and the nanocomposites were consolidated using rapid high-frequency induction heat sintering route. The resulting nanocomposites demonstrated higher mechanical properties due to efficient GNS incorporation and chemical interaction with the Al2O3 matrix grains. The enhancement in mechanical properties is attributed to (i) uniformly-dispersed GNS in the consolidated structure (ii) ability of GNS to decorate Al2O3 nanoparticles and (iii) strong GNS/Al2O3 chemical interaction during colloidal mixing and pullout/crack bridging toughening mechanisms during mechanical testing. The GNS/Al2O3 interaction during different processing stages was thoroughly examined by thermal and structural investigation of the interfacial area. The formation of an intermediate aluminum oxycarbide phase (Al2OC) via a confined carbothermal reduction reaction at the GNS/Al2O3 interface was observed using advanced electron microscopes. The GNS surface roughness improves GNS/Al2O3 mechanical locking and chemical compatibility. The sturdy interface phase facilitates efficient load transfer and delayed failure through impediment of crack propagation. The resulting nanocomposites, therefore, offer superior toughness.

Keywords: ceramics, nanocomposites, interfaces, nanostructures, electron microscopy, Al2O3

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Authors: Hyunho Shin, Jaekwang Jung, Jeongho Park, Sungwon Hwang

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For the application of graphene quantum dots (GQDs) to optoelectronic nanodevices, it is of critical importance to understand the mechanisms which result in novel phenomena of their light absorption/emission. The optical transitions are known to be available up to ~6 eV in GQDs, especially useful for ultraviolet (UV) photodetectors (PDs). Here, we present size-dependent shape/edge-state variations of GQDs and visible photoluminescence (PL) showing anomalous size dependencies. With varying the average size (da) of GQDs from 5 to 35 nm, the peak energy of the absorption spectra monotonically decreases, while that of the visible PL spectra unusually shows nonmonotonic behaviors having a minimum at diameter ∼17 nm. The PL behaviors can be attributed to the novel feature of GQDs, that is, the circular-to-polygonal-shape and corresponding edge-state variations of GQDs at diameter ∼17 nm as the GQD size increases, as demonstrated by high resolution transmission electron microscopy. We believe that such a comprehensive scheme in designing device architecture and the structural formulation of GQDs provides a device for practical realization of environmentally benign, high performance flexible devices in the future.

Keywords: graphene, quantum dot, size, photoluminescence

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Authors: Khiaira S. Hassan, Abbas S. Alwan, Muna K. Abbass

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This research aims to study the effect of the liquid nitriding and shot peening on the hardness, surface roughness, residual stress, microstructure and corrosion behavior of austenite stainless steel 316 L. Chemical surface heat treatment by liquid nitriding process was carried out at 500 °C for 1 h and followed by shot peening with using ball steel diameter of 1.25 mm in different exposure time of 10 and 20 min. Electrochemical corrosion test was applied in sea water (3.5% NaCl solution) by using potentostat instrument. The results showed that the nitride layer consists of a compound layer (white layer) and diffusion zone immediately below the alloy layer. It has been found that the mechanical treatment (shot peening) has led to the formation of compressive residual stresses in layer surface that increased the hardness of stainless steel surface. All surface treatment (nitriding and shot peening) processes have led to the formation of carbide of CrN in hard surface layer. It was shown that both processes caused an increase in surface hardness and roughness which increases with shot peening time. Also, the corrosion results showed that the liquid nitriding and shot peening processes increase the corrosion rate to values more than that of not treated stainless steel.

Keywords: stainless steel 316L, shot peening, nitriding, corrosion, hardness

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Authors: Laroussi Chaabane, Amel El Ghali, Emmanuel Beyou, Mohamed Hassen V. Baouab

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In this research, the functionalization of graphene oxide sheets by ethylenediamine (EDA) was accomplished and followed by the grafting of bis(2-pyridylmethyl) amino group (BPED) onto the activated graphene oxide sheets in the presence of chloroacetylchloride (CAC) and then combined with magnetic nanoparticles (Fe₃O₄NPs) to produce a magnetic graphene-based composite [(Go-EDA-CAC)@Fe₃O₄NPs-BPED]. The physicochemical properties of [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] composites were investigated by Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA). Additionally, the catalysts can be easily recycled within ten seconds by using an external magnetic field. Moreover, [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] was used for removing Cu(II) ions from aqueous solutions using a batch process. The effect of pH, contact time and temperature on the metal ions adsorption were investigated, however weakly dependent on ionic strength. The maximum adsorption capacity values of Cu(II) on the [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] at the pH of 6 is 3.46 mmol.g⁻¹. To examine the underlying mechanism of the adsorption process, pseudo-first, pseudo-second-order, and intraparticle diffusion models were fitted to experimental kinetic data. Results showed that the pseudo-second-order equation was appropriate to describe the Cu (II) adsorption by [(Go-EDA-CAC)@Fe₃O₄NPs-BPED]. Adsorption data were further analyzed by the Langmuir, Freundlich, and Jossens adsorption approaches. Additionally, the adsorption properties of the [(Go-EDA-CAC)@Fe₃O₄NPs-BPED], their reusability (more than 6 cycles) and durability in the aqueous solutions open the path to removal of Cu(II) from water solution. Based on the results obtained, we report the activity of Cu(II) supported on [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] as a catalyst for the cross-coupling of symmetric alkynes.

Keywords: graphene, magnetic nanoparticles, adsorption kinetics/isotherms, cross coupling

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Authors: Xi Wang, Yoshio Bando

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Lithium-ion batteries (LIBs) can deliver high levels of energy storage density and offer long operating lifetimes, but their power density is too low for many important applications. Therefore, we developed some new strategies and fabricated novel electrodes for fast Li transport and its facile synthesis including N-doped graphene-SnO2 sandwich papers, bicontinuous nanoporous Cu/Li4Ti5O12 electrode, and binder-free N-doped graphene papers. In addition, by using advanced in-TEM, STEM techniques and the theoretical simulations, we systematically studied and understood their storage mechanisms at the atomic scale, which shed a new light on the reasons of the ultrafast lithium storage property and high capacity for these advanced anodes. For example, by using advanced in-situ TEM, we directly investigated these processes using an individual CuO nanowire anode and constructed a LIB prototype within a TEM. Being promising candidates for anodes in lithium-ion batteries (LIBs), transition metal oxide anodes utilizing the so-called conversion mechanism principle typically suffer from the severe capacity fading during the 1st cycle of lithiation–delithiation. Also we report on the atomistic insights of the GN energy storage as revealed by in situ TEM. The lithiation process on edges and basal planes is directly visualized, the pyrrolic N "hole" defect and the perturbed solid-electrolyte-interface (SEI) configurations are observed, and charge transfer states for three N-existing forms are also investigated. In situ HRTEM experiments together with theoretical calculations provide a solid evidence that enlarged edge {0001} spacings and surface "hole" defects result in improved surface capacitive effects and thus high rate capability and the high capacity is owing to short-distance orderings at the edges during discharging and numerous surface defects; the phenomena cannot be understood previously by standard electron or X-ray diffraction analyses.

Keywords: in-situ TEM, STEM, advanced anode, lithium-ion batteries, storage mechanism

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Authors: Wei-Song Hung

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We utilized pressure, vacuum, and evaporation-assisted self-assembly techniques through which graphene oxide (GO) was deposited on modified polyacrylonitrile (mPAN). The fabricated composite GO/mPAN membranes were applied to dehydrate 1-butanol mixtures by pervaporation. Varying driving forces in the self-assembly techniques induced different GO assembly layer microstructures. XRD results indicated that the GO layer d-spacing varied from 8.3 Å to 11.5 Å. The self-assembly technique with evaporation resulted in a heterogeneous GO layer with loop structures; this layer was shown to be hydrophobic, in contrast to the hydrophilic layer formed from the other two techniques. From the pressure-assisted technique, the composite membrane exhibited exceptional pervaporation performance at 30 C: concentration of water at the permeate side = 99.6 wt% and permeation flux = 2.54 kg m-2 h-1. Moreover, the membrane sustained its operating stability at a high temperature of 70 C: a high water concentration of 99.5 wt% was maintained, and a permeation flux as high as 4.34 kg m-2 h-1 was attained. This excellent separation performance stemmed from the dense, highly ordered laminate structure of GO.

Keywords: graphene oxide, self-assembly, alcohol dehydration, polyacrylonitrile (mPAN)

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Authors: M. A. Kassim, R. Potumarthi, A. Tanksale, S. C. Srivatsa, S. Bhattacharya

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Enzymatic saccharification of biomass for reducing sugar production is one of the crucial processes in biofuel production through biochemical conversion. In this study, enzymatic saccharification of dilute potassium hydroxide (KOH) pre-treated Tetraselmis suecica biomass was carried out by using cellulase enzyme obtained from Trichoderma longibrachiatum. Initially, the pre-treatment conditions were optimised by changing alkali reagent concentration, retention time for reaction, and temperature. The T. suecica biomass after pre-treatment was also characterized using Fourier Transform Infrared Spectra and Scanning Electron Microscope. These analyses revealed that the functional group such as acetyl and hydroxyl groups, structure and surface of T. suecica biomass were changed through pre-treatment, which is favourable for enzymatic saccharification process. Comparison of enzymatic saccharification of untreated and pre-treated microalgal biomass indicated that higher level of reducing sugar can be obtained from pre-treated T. suecica. Enzymatic saccharification of pre-treated T. suecica biomass was optimised by changing temperature, pH, and enzyme concentration to solid ratio ([E]/[S]). Highest conversion of carbohydrate into reducing sugar of 95% amounted to reducing sugar yield of 20 (wt%) from pre-treated T. suecica was obtained from saccharification, at temperature: 40°C, pH: 4.5 and [E]/[S] of 0.1 after 72 h of incubation. Hydrolysate obtained from enzymatic saccharification of pretreated T. suecica biomass was further fermented into biobutanol using Clostridium saccharoperbutyliticum as biocatalyst. The results from this study demonstrate a positive prospect of application of dilute alkaline pre-treatment to enhance enzymatic saccharification and biobutanol production from microalgal biomass.

Keywords: microalgal biomass, enzymatic saccharification, biobutanol, fermentation

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Authors: Jhen-Ting Huang, Chia-Chia Chang, Hu-Cheng Weng, An-Ya Lo

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In this study, Co3O4-CNT-Graphene composite electrode was deposited by electrophoretic deposition (EPD) method, where micro polystyrene spheres (PSs) were added for co-deposition. Applied with heat treatment, a hierarchical porosity is left in the electrode which is beneficial for supercapacitor application. In terms of charge and discharge performance, we discussed the optimal CNT/Graphene ratio, macroporous ratio, and the effect of Co3O4 addition on electrode capacitance. For materials characterization, scanning electron microscope (SEM), X-ray diffraction, and BET were applied, while cyclic voltammetry (CV) and chronopotentiometry (CP) measurements, and Ragone plot were applied as in-situ analyses. Based on this, the effects of PS amount on the structure, porosity and their effect on capacitance of the electrodes were investigated. Finally, the full device performance was examined with charge-discharge and electron impedance spectrum (EIS) methods. The results show that the EPD coating with hierarchical porosity was successfully demonstrated in this study. As a result, the capacitance was greatly enhanced by 2.6 times with the hierarchical structure.

Keywords: supercapacitor, nanocarbon tub, graphene, metal oxide

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Authors: Anna V. Zaporozhchenko, Dmytro Kutnyakhov, Katherina Medjanik, Christian Tusche, Hans-Joachim Elmers, Olena Fedchenko, Sergey Chernov, Martin Ellguth, Sergej A. Nepijko, Gerd Schoenhense

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Graphene reveals a unique electronic structure that predetermines many intriguing properties such as massless charge carriers, optical transparency and high velocity of fermions at the Fermi level, opening a wide horizon of future applications. Hence, a detailed investigation of the electronic structure of graphene is crucial. The method of choice is angular resolved photoelectron spectroscopy ARPES. Here we present experiments using time-of-flight (ToF) momentum microscopy, being an alternative way of ARPES using full-field imaging of the whole Brillouin zone (BZ) and simultaneous acquisition of up to several 100 energy slices. Unlike conventional ARPES, k-microscopy is not limited in simultaneous k-space access. We have recorded the whole first BZ of graphene on Ir(111) including all six Dirac cones. As excitation source we used synchrotron radiation from BESSY II (Berlin) at the U125-2 NIM, providing linearly polarized (both polarizations p- and s-) VUV radiation. The instrument uses a delay-line detector for single-particle detection up the 5 Mcps range and parallel energy detection via ToF recording. In this way, we gather a 3D data stack I(E,kx,ky) of the full valence electronic structure in approx. 20 mins. Band dispersion stacks were measured in the energy range of 14 eV up to 23 eV with steps of 1 eV. The linearly-dispersing graphene bands for all six K and K’ points were simultaneously recorded. We find clear features of hybridization with the substrate, in particular in the linear dichroism in the angular distribution (LDAD). Recording of the whole Brillouin zone of graphene/Ir(111) revealed new features. First, the intensity differences (i.e. the LDAD) are very sensitive to the interaction of graphene bands with substrate bands. Second, the dark corridors are investigated in detail for both, p- and s- polarized radiation. They appear as local distortions of photoelectron current distribution and are induced by quantum mechanical interference of graphene sublattices. The dark corridors are located in different areas of the 6 Dirac cones and show chirality behaviour with a mirror plane along vertical axis. Moreover, two out of six show an oval shape while the rest are more circular. It clearly indicates orientation dependence with respect to E vector of incident light. Third, a pattern of faint but very sharp lines is visible at energies around 22eV that strongly remind on Kikuchi lines in diffraction. In conclusion, the simultaneous study of all six Dirac cones is crucial for a complete understanding of dichroism phenomena and the dark corridor.

Keywords: band structure, graphene, momentum microscopy, LDAD

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Authors: Vishal V. R. Nandigana, Mohammad Heiranian, Narayana R. Aluru

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Graphene material has found tremendous applications in water desalination, DNA sequencing and energy storage. Multiple nanopores are etched to create opening for water desalination and energy storage applications. The nanopores created are of the order of 3-5 nm allowing multiple ions to transport through the pore. In this paper, we present for the first time, molecular dynamics study of single ion transport, where only one ion passes through the graphene nanopore. The diameter of the graphene nanopore is of the same order as the hydration layers formed around each ion. Analogous to single electron transport resulting from ionic transport is observed for the first time. The current-voltage characteristics of such a device are similar to single electron transport in quantum dots. The current is blocked until a critical voltage, as the ions are trapped inside a hydration shell. The trapped ions have a high energy barrier compared to the applied input electrical voltage, preventing the ion to break free from the hydration shell. This region is called “Coulomb blockade region”. In this region, we observe zero transport of ions inside the nanopore. However, when the electrical voltage is beyond the critical voltage, the ion has sufficient energy to break free from the energy barrier created by the hydration shell to enter into the pore. Thus, the input voltage can control the transport of the ion inside the nanopore. The device therefore acts as a binary storage unit, storing 0 when no ion passes through the pore and storing 1 when a single ion passes through the pore. We therefore postulate that the device can be used for fluidic computing applications in chemistry and biology, mimicking a computer. Furthermore, the trapped ion stores a finite charge in the Coulomb blockade region; hence the device also acts a super capacitor.

Keywords: graphene nanomembrane, single ion transport, Coulomb blockade, nanofluidics

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Authors: Gulcin Yildiz, Hao Feng

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In recent years there is growing interested in using soy protein because of several advantages compared to other protein sources, such as high nutritional value, steady supply, and low cost. Soy protein isolate (SPI) is the most refined soy protein product. It contains 90% protein in a moisture-free form and has some desirable functionalities. Creating a protein-polysaccharide conjugate to be the emulsifying agent rather than the protein alone can markedly enhance its stability. This study was undertaken to examine the effects of ultrasound treatments on the physicochemical properties of SPI-starch conjugates. The soy protein isolate (SPI, Pro-Fam® 955) samples were obtained from the Archer Daniels Midland Company. Protein concentrations were analyzed by the Bardford method using BSA as the standard. The volume-weighted mean diameters D [4,3] of protein–polysaccharide conjugates were measured by dynamic light scattering (DLS). Surface hydrophobicity of the conjugates was measured by using 1-anilino-8-naphthalenesulfonate (ANS) (Sigma-Aldrich, St. Louis, MO, USA). Increasing the pH from 2 to 12 resulted in increased protein solubility. The highest solubility was 69.2% for the sample treated with ultrasonication at pH 12, while the lowest (9.13%) was observed in the Control. For the other pH conditions, the protein solubility values ranged from 40.53 to 49.65%. The ultrasound treatment significantly decreased the particle sizes of the SPI-modified starch conjugates. While the D [4,3] for the Control was 731.6 nm, it was 293.7 nm for the samples treated by sonication at pH 12. The surface hydrophobicity (H0) of SPI-starch at all pH conditions were significantly higher than those in the Control. Ultrasonication was proven to be effective in improving the solubility and emulsifying properties of soy protein isolate-starch conjugates.

Keywords: particle size, solubility, soy protein isolate, ultrasonication

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Authors: Ko-Shao Chen, Yun Tsao, Chia-Hsuan Tsen, Chien-Chung Chen, Shu-Chuan Liao

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Electrospun microtube array membranes (MTAMs) made of PLLA (poly-L-lactic acid) have wide potential applications in tissue engineering. However, their surface hydrophobicity and poor biocompatability have limited their further usage. In this study, the surface of PLLA MTAMs were made hydrophilic by introducing extra functional groups, such as peroxide, via an acetic acid plasma (AAP). UV-graft polymerization of acrylic acid (G-AAc) was then used to produce carboxyl group on MTAMs surface, which bonded covalently with chitosan through EDC / NHS crosslinking agents. To evaluate the effects of the surface modification on PLLA MTAMs, water contact angle (WCA) measurement and cell compatibility tests were carried out. We found that AAP treated electrospun PLLA MTAMs grafted with AAc and, finally, with chitosan immobilized via crosslinking agent, exhibited improved hydrophilic and cell compatibility.

Keywords: plasma, EDC/NHS, UV grafting, Chitosan, microtube array membrane (MTAMs)

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Authors: Rashad Al-Gaashani, Muataz A. Atieh

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In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

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Authors: Pinki Sharma, Himanshu Joshi

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Distillery spentwash contains high chemical oxygen demand (COD), biological oxygen demand (BOD), color, total dissolved solids (TDS) and other contaminants even after biological treatment. The effluent can’t be discharged as such in the surface water bodies or land without further treatment. Reverse osmosis (RO) treatment plants have been installed in many of the distilleries at tertiary level. But at most of the places these plants are not properly working due to high concentration of organic matter and other contaminants in biologically treated spentwash. To make the membrane treatment proven and reliable technology, proper pre-treatment is mandatory. In the present study, ultra-filtration (UF) as pre-treatment of RO at tertiary stage was performed. Operating parameters namely initial pH (pHo: 2–10), trans-membrane pressure (TMP: 4-20 bars) and temperature (T: 15- 43°C) used for conducting experiments with UF system. Experiments were optimized at different operating parameters in terms of COD, color, TDS and TOC removal by using response surface methodology (RSM) with central composite design. The results showed that removal of COD, color and TDS by 62%, 93.5% and 75.5%, with UF, respectively at optimized conditions with increased permeate flux from 17.5 l/m2/h (RO) to 38 l/m2/h (UF-RO). The performance of the RO system was greatly improved both in term of pollutant removal as well as water recovery.

Keywords: bio-digested distillery spentwash, reverse osmosis, response surface methodology, ultra-filtration

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Authors: Sudkate Chaiyo, Weena Siangproh, Orawon Chailapakul, Kurt Kalcher

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In the present work, a simple and sensitive non-enzymatic electrochemical detection of glucose in disposable paper-based sensor was developed at ionic liquid/graphene/cobalt phthalocyanine composite (IL/G/CoPc) modified electrode. The morphology of the fabricated composite was characterized and confirmed by scanning electron microscopy and UV-Vis spectroscopy. The UV-Vis spectroscopy results confirmed that the G/CoPc composite formed via the strong π–π interaction between CoPc and G. Amperometric i-t technique was used for the determination of glucose. The response of glucose was linear over the concentration ranging from 10 µM to 1.5 mM. The response time of the sensor was found as 30 s with a limit of detection of 0.64 µM (S/N=3). The fabricated sensor also exhibited its good selectivity in the presence of common interfering species. In addition, the fabricated sensor exhibited its special advantages such as low working potential, good sensitivity along with good repeatability and reproducibility for the determination of glucose.

Keywords: glucose, paper-based sensor, ionic liquid/graphene/cobalt phthalocyanine composite, electrochemical detection

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Authors: A. M. Iordache, S. M. Iordache, V. Barna, M. Elisa, I. C. Vasiliu, C. R. Stefan, I. Chilibon, I. Stamatin, S. Caramizoiu, C. E. A. Grigorescu

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The general objective of the presentation is the development of an e-tongue like sensor based on modified screen printed electrode (SPE) structures with a receptor part made of porphyrins/metalloporphyrins chemically bound to graphene (the sensitive assembly) to act as antennas and “capture” the histamine molecules. Using a single, ultra-sensitive electrochemical sensor, we measured the concentration of histamine, a compound which is strongly connected to the level of freshness in foods (the caution level of histamine is 50 ppm, whereas the maximum accepted levels range from 200 ppm to 500 ppm). Our approach for the chemical immobilization of the porphyrins onto the surface of the graphenes was via substitution reaction: a solution of graphene in SOCl2 was heated to 800C for 6 hours. Upon cooling, the metallo-porphyrins were added and ultrasonicated for 4 hours. The solution was then allowed to cool to room temperature and then centrifuged in order to separate the deposit. The sensitive assembly was drop casted onto the carbon SPE and cyclic voltammetry was performed in the presence of histamine. The reaction is quasi-reversible and the sensor showed an oxidation potential for histamine at 600 mV. The results indicate a linear dependence of concentration of histamine as function of intensity. The results are reproducible; however the chemical stability of the sensitive assembly is low.

Keywords: histamine, cyclic voltammetry, metallo-porphyrin, food freshness

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Authors: M. A. Moussa, M. H. Abdel Rehim, G.M. Turky

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Polyaniline composites with carbon nitride, to overcome compatibility restriction with graphene, were prepared with the solution method. FTIR and Uv-vis spectra were used for structural conformation. While XRD and XPS confirmed the structures in addition to estimation of nitrogen atom surroundings, the pore sizes and the active surface area were determined from BET adsorption isotherm. The electrical and dielectric parameters were measured and calculated with BDS .

Keywords: carbon nitride, dynamic relaxation, electrical conductivity, polyaniline

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Authors: Rafael do Amaral Teodoro, Leandro Augusto da Silva

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Originated from graphite, graphene is a two-dimensional (2D) material that promises to revolutionize technology in many different areas, such as energy, telecommunications, civil construction, aviation, textile, and medicine. This is possible because its structure, formed by carbon bonds, provides desirable optical, thermal, and mechanical characteristics that are interesting to multiple areas of the market. Thus, several research and development centers are studying different manufacturing methods and material applications of graphene, which are often compromised by the scarcity of more agile and accurate methodologies to characterize the material – that is to determine its composition, shape, size, and the number of layers and crystals. To engage in this search, this study proposes a computational methodology that applies deep learning to identify graphene oxide crystals in order to characterize samples by crystal sizes. To achieve this, a fully convolutional neural network called U-net has been trained to segment SEM graphene oxide images. The segmentation generated by the U-net is fine-tuned with a standard deviation technique by classes, which allows crystals to be distinguished with different labels through an object delimitation algorithm. As a next step, the characteristics of the position, area, perimeter, and lateral measures of each detected crystal are extracted from the images. This information generates a database with the dimensions of the crystals that compose the samples. Finally, graphs are automatically created showing the frequency distributions by area size and perimeter of the crystals. This methodological process resulted in a high capacity of segmentation of graphene oxide crystals, presenting accuracy and F-score equal to 95% and 94%, respectively, over the test set. Such performance demonstrates a high generalization capacity of the method in crystal segmentation, since its performance considers significant changes in image extraction quality. The measurement of non-overlapping crystals presented an average error of 6% for the different measurement metrics, thus suggesting that the model provides a high-performance measurement for non-overlapping segmentations. For overlapping crystals, however, a limitation of the model was identified. To overcome this limitation, it is important to ensure that the samples to be analyzed are properly prepared. This will minimize crystal overlap in the SEM image acquisition and guarantee a lower error in the measurements without greater efforts for data handling. All in all, the method developed is a time optimizer with a high measurement value, considering that it is capable of measuring hundreds of graphene oxide crystals in seconds, saving weeks of manual work.

Keywords: characterization, graphene oxide, nanomaterials, U-net, deep learning

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Authors: Sukla Saha, Alok Sinha

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Acid mine drainage (AMD) is the generation of acidic water from active as well as abandoned mines. AMD generates due to the oxidation of pyrites present in the rock in mining areas. Sulfur oxidizing bacteria such as Thiobacillus ferrooxidans acts as a catalyst in this oxidation process. The characteristics of AMD is extreme low pH (2-3) with elevated concentration of different heavy metals such as Fe, Al, Zn, Mn, Cu and Co and anions such sulfate and chloride. AMD contaminate the ground water as well as surface water which leads to the degradation of water quality. Moreover, it carries detrimental effect for aquatic organism and degrade the environment. In the present study, AMD is treated with fly ash, modified with alkaline agent (NaOH). This modified fly ash (MFA) was experimentally proven as a very effective neutralizing agent for the treatment of AMD. It was observed that pH of treated AMD raised to 9.22 from 1.51 with 100g/L of MFA dose. Approximately, 99% removal of Fe, Al, Mn, Cu and Co took place with the same MFA dose. The treated water comply with the effluent discharge standard of (IS: 2490-1981).

Keywords: acid mine drainage, heavy metals, modified fly ash, neutralization

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Authors: Mahtab Assadian, Mohd Hasbullah Idris, Mostafa Rezazadeh Shirdar, Mohammad Mahdi Taheri, ‎S. Izman

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Corrosion behaviour and surface roughness of magnesium substrate were investigated after NaOH pretreatment in different concentrations (1, 5, and 10 molar) and duration of (10 min, 30 min, 1 h, 3 h, 6 h and 24 h). Creation of Mg(OH)2 barrier layer after pretreatment enhanced corrostion resistance as well as wettability of substrate surface. Characterization including Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) was conducted to detect the existence of this barrier layer. Surface roughness and wettability of substrate was evaluated using atomic force microscopy (AFM) and contact angle measurement respectively. It is found that magnesium treated by 1M NaOH for 30 min reveals higher corrosion resistance and lower water contact angle of substrate surface. In addition, this investigation indicates that pH value of SBF solution is strongly influenced by different time and concentration of alkaline pretreatment.

Keywords: magnesium, NaOH pretreatment, corrosion resistance, wettability

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Authors: Štěpán Hýsek, Petra Gajdačová, Milan Podlena

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Annual plants are becoming more and more popular source of lignin and cellulose. In those days a lot of research is carried out in order to evaluate the possibility of utilization of fibres and particles from these plants in composite materials production. These lingo-cellulosic materials seem to be a great alternative to wood, however, due to waxy and silica layers on the surface of these stalks, one additional technological step is needed–erosion of the layers for the purpose of achieving better adhesion between particle and adhesive. In this research, we used several kinds of particle pre-treatment, in order to modify surface properties of these particles. Further, an adhesive was applied to the particles using laboratory blender and board were produced using laboratory press. Both physical and mechanical properties of boards were observed. It was found out that the surface modification of particles had statistically significant effect on properties of produced boards.

Keywords: annual plant, composites, mechanical properties, particleboard

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Authors: Biswaranjan D. Mohapatra, Ipsha Hota, Swarna P. Mantry, Nibedita Behera, Kumar S. K. Varadwaj

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Designing highly active and low-cost oxygen evolution (2H₂O → 4H⁺ + 4e⁻ + O₂) electrocatalyst is one of the most active areas of advanced energy research. Some precious metal-based electrocatalysts, such as IrO₂ and RuO₂, have shown excellent performance for oxygen evolution reaction (OER); however, they suffer from high-cost and low abundance which limits their applications. Recently, layered double hydroxides (LDHs), composed of layers of divalent and trivalent transition metal cations coordinated to hydroxide anions, have gathered attention as an alternative OER catalyst. However, LDHs are insulators and coupled with carbon materials for the electrocatalytic applications. Graphene covalently doped with nitrogen has been demonstrated to be an excellent electrocatalyst for energy conversion technologies such as; oxygen reduction reaction (ORR), oxygen evolution reaction (OER) & hydrogen evolution reaction (HER). However, they operate at high overpotentials, significantly above the thermodynamic standard potentials. Recently, we reported remarkably enhanced catalytic activity of benzoate or 1-pyrenebutyrate functionalized N-doped graphene towards the ORR in alkaline medium. The molecular and heteroatom co-doping on graphene is expected to tune the electronic structure of graphene. Therefore, an innovative catalyst architecture, in which LDHs are anchored on aromatic acid functionalized ‘N’ doped graphene may presumably boost the OER activity to a new benchmark. Herein, we report fabrication of Co₂Fe-LDH on aromatic acid (AA) functionalized ‘N’ doped reduced graphene oxide (NG) and studied their OER activities in alkaline medium. In the first step, a novel polyol method is applied for synthesis of AA functionalized NG, which is well dispersed in aqueous medium. In the second step, Co₂Fe LDH were grown on AA functionalized NG by co-precipitation method. The hybrid samples are abbreviated as Co₂Fe LDH/AA-NG, where AA is either Benzoic acid or 1, 3-Benzene dicarboxylic acid (BDA) or 1, 3, 5 Benzene tricarboxylic acid (BTA). The crystal structure and morphology of the samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). These studies confirmed the growth of layered single phase LDH. The electrocatalytic OER activity of these hybrid materials was investigated by rotating disc electrode (RDE) technique on a glassy carbon electrode. The linear sweep voltammetry (LSV) on these catalyst samples were taken at 1600rpm. We observed significant OER performance enhancement in terms of onset potential and current density on Co₂Fe LDH/BTA-NG hybrid, indicating the synergic effect. This exploration of molecular functionalization effect in doped graphene and LDH system may provide an excellent platform for innovative design of OER catalysts.

Keywords: π-π functionalization, layered double hydroxide, oxygen evolution reaction, reduced graphene oxide

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Authors: Sundaram Chandrasekaran, Seung Hyun Hur

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Exploring strategies for oxygen vacancy engineering under mild conditions and understanding the relationship between dislocations and photoelectrochemical (PEC) cell performance are challenging issues for designing high performance PEC devices. Therefore, it is very important to understand that how the oxygen vacancies (VO) or other defect states affect the performance of the photocatalyst in photoelectric transfer. So far, it has been found that defects in nano or micro crystals can have two possible significances on the PEC performance. Firstly, an electron-hole pair produced at the interface of photoelectrode and electrolyte can recombine at the defect centers under illumination of light, thereby reducing the PEC performances. On the other hand, the defects could lead to a higher light absorption in the longer wavelength region and may act as energy centers for the water splitting reaction that can improve the PEC performances. Even if the dislocation growth of ZnO has been verified by the full density functional theory (DFT) calculations and local density approximation calculations (LDA), it requires further studies to correlate the structures of ZnO and PEC performances. Exploring the hybrid structures composed of graphene oxide (GO) and ZnO nanostructures offer not only the vision of how the complex structure form from a simple starting materials but also the tools to improve PEC performances by understanding the underlying mechanisms of mutual interactions. As there are few studies for the ZnO growth with other materials and the growth mechanism in those cases has not been clearly explored yet, it is very important to understand the fundamental growth process of nanomaterials with the specific materials, so that rational and controllable syntheses of efficient ZnO-based hybrid materials can be designed to prepare nanostructures that can exhibit significant PEC performances. Herein, we fabricated various ZnO nanostructures such as hollow sphere, bucky bowl, nanorod and triangle, investigated their pH dependent growth mechanism, and correlated the PEC performances with them. Especially, the origin of well-controlled dislocation-driven growth and its transformation mechanism of ZnO nanorods to triangles on the GO surface were discussed in detail. Surprisingly, the addition of GO during the synthesis process not only tunes the morphology of ZnO nanocrystals and also creates more oxygen vacancies (oxygen defects) in the lattice of ZnO, which obviously suggest that the oxygen vacancies be created by the redox reaction between GO and ZnO in which the surface oxygen is extracted from the surface of ZnO by the functional groups of GO. On the basis of our experimental and theoretical analysis, the detailed mechanism for the formation of specific structural shapes and oxygen vacancies via dislocation, and its impact in PEC performances are explored. In water splitting performance, the maximum photocurrent density of GO-ZnO triangles was 1.517mA/cm-2 (under UV light ~ 360 nm) vs. RHE with high incident photon to current conversion Efficiency (IPCE) of 10.41%, which is the highest among all samples fabricated in this study and also one of the highest IPCE reported so far obtained from GO-ZnO triangular shaped photocatalyst.

Keywords: dislocation driven growth, zinc oxide, graphene oxide, water splitting

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Authors: Laroussi Chaabane, Emmanuel Beyou, Amel El Ghali, Mohammed Hassen V. Baouab

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The functionalization of graphene oxide sheets by ethylenediamine (EDA) was accomplished followed by the grafting of bis(2-pyridylmethyl)amino group (BPED) onto the activated graphene oxide sheets in the presence of chloroacetylchloride (CAC) produced the martial [(Go-EDA-CAC)-BPED]. The physic-chemical properties of [(Go-EDA-CAC)-BPED] composites were investigated by Fourier transform infrared (FT-IR), X-ray photoelectron spectroscopy (XPs), Scanning electron microscopy (SEM) and Thermogravimetric analysis (TGA). Moreover, [(Go-EDA-CAC)-BPED] was used for removing M(II) (where M=Cu, Ni and Co) ions from aqueous solutions using a batch process. The effect of pH, contact time and temperature were investigated. More importantly, the [(Go-EDA-CAC)-BPED] adsorbent exhibited remarkable performance in capturing heavy metal ions from water. The maximum adsorption capacity values of Cu(II), Ni(II) and Co(II) on the [(GO-EDA-CAC)-BPED] at the pH of 7 is 3.05 mmol.g⁻¹, 3.25 mmol.g⁻¹ and 3.05 mmol.g⁻¹ respectively. To examine the underlying mechanism of the adsorption process, pseudo-first, pseudo-second-order, and intraparticle diffusion models were fitted to experimental kinetic data. Results showed that the pseudo-second-order equation was appropriate to describe the three metal ions adsorption by [(Go-EDA-CAC)-BPED]. Adsorption data were further analyzed by the Langmuir, Freundlich, and Jossensadsorption approaches. Additionally, the adsorption properties of the [(Go-EDA-CAC)-BPED], their reusability (more than 10 cycles) and durability in the aqueous solutions open the path to removal of metal ions (Cu(II), Ni(II) and Co(II) from water solution. Based on the results obtained, we conclude that [(Go-EDA-CAC)-BPED] can be an effective and potential adsorbent for removing metal ions from an aqueous solution.

Keywords: graphene oxide, bis(2-pyridylmethyl)amino, adsorption kinetics, isotherms

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Authors: Ahmad Amiri, Hamed K. Arzani, S. N. Kazi, B. T. Chew

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Since graphene nanoplatelet (GNP) is a promising material due to desirable thermal properties, this paper is related to the thermophysical and heat transfer performance of covalently functionalized GNP-based water/ethylene glycol nanofluid through an annular channel. After experimentally measuring thermophysical properties of prepared samples, a computational fluid dynamics study has been carried out to examine the heat transfer and pressure drop of well-dispersed and stabilized nanofluids. The effect of concentration of GNP and Reynolds number at constant wall temperature boundary condition under turbulent flow regime on convective heat transfer coefficient has been investigated. Based on the results, for different Reynolds numbers, the convective heat transfer coefficient of the prepared nanofluid is higher than that of the base fluid. Also, the enhancement of convective heat transfer coefficient and thermal conductivity increase with the increase of GNP concentration in base-fluid. Based on the results of this investigation, there is a significant enhancement on the heat transfer rate associated with loading well-dispersed GNP in base-fluid.

Keywords: nanofluid, turbulent flow, forced convection flow, graphene, annular, annulus

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Authors: Kiran Roat, Bhanupriya Sanger, Gayatri Swarnakar

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Amphistomiasis disease is the main health problem throughout of the world and responsible for great economic losses to cattle industries, mostly to poor cattle farmers in developing countries. Among the rumen parasites, the Paramphistomum cervi were collected from the rumen of freshly slaughtered buffalo for the further treatment process. Trigonella foenum-graecum is commonly known as methi and fenugreek and their seeds are known for their therapeutic value. The present study was considered to evaluate in vitro efficacy of aqueous extract of Trigonella foenum-graecum on P. cervi. 130 mg/ml concentration of aqueous extract shows total mortality of P. cervi at 5 hours. The ultrastructural surface topography of untreated animal was compared with a treated animal by scanning electron microscope (SEM). The body of untreated P. cervi in conical shape, tegumental surface is highly ridged with transverse folds and present abundance number of papillaes. Observations demonstrated that the body of treated P. cervi become shrunken & elongated. Treated parasite shows the deep breakage in tegument and the disappearance of tegumental folds & papillae. Severe blebs formations have been found. Above findings, it can be concluded that the seeds of Trigonella foenum-graecum can be used as an anthelminthic agent to eliminate P. cervi from the body of buffalo.

Keywords: Paramphistomum cervi, Trigonella foenum-graecum, scanning electron microscope, buffalo

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