Search results for: polymer chemistry

Authors: Salwa M. Elmesallamy, Ahmed A. Farag, Magd M. Badr, Dalia S. Fathy, Ahmed Bakry, Mona A. El-Etre

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The term green environment is an international trend. It is become imperative to treat the corrosion of steel with a green coating to protect the environment. From the potential adverse effects of the traditional materials.A series of polybenzoxazine/henna composites (PBZ/henna), with different weight percent (3,5, and 7 wt % (of henna), were prepared for corrosion protection of carbon steel. The structures of the prepared composites were verified using FTIR analysis. The mechanical properties of the resins, such as adhesion, hardness, binding, and tensile strength, were also measured. It was found that the tensile strength increases by henna loading up to 25% higher than the tidy resin. The thermal stability was investigated by thermogravimetric analysis (TGA) the loading of lawsone (henna) molecules into the PBZ matrix increases the thermal stability of the composite. UV stability was tested by the UV weathering accelerator to examine the possibility that henna can also act as an aging UV stabilizer. The effect of henna content on the corrosion resistance of composite coatings was tested using potentiostatic polarization and electrochemical spectroscopy. The presence of henna in the coating matrix enhances the protection efficiency of polybenzoxazine coats. Increasing henna concentration increases the protection efficiency of composites. The quantum chemical calculations for polybenzoxazine/henna composites have resulted that the highest corrosion inhibition efficiency, has the highest EHOMO and lowest ELUMO; which is in good agreement with results obtained from experiments.

Keywords: polybenzoxazine, corrosion, green chemistry, carbon steel

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Authors: Viriyavudh Sim, SeungHyun Kim, JungKyu Choi, WooYoung Jung

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Glass Fiber Reinforced Polymer (GFRP) is a major evolution for energy dissipation when used as infill material for seismic retrofitting of steel frame, a basic PMC infill wall system consists of two GFRP laminates surrounding an infill of foam core. This paper presents numerical analysis in terms of buckling resistance of GFRP sandwich infill panels system under the influence of environment temperature and stacking sequence of laminate skin. Mode of failure under in-plane compression is studied by means of numerical analysis with ABAQUS platform. Parameters considered in this study are contact length between infill and frame, laminate stacking sequence of GFRP skin and variation of mechanical properties due to increment of temperature. The analysis is done with four cases of simple stacking sequence over a range of temperature. The result showed that both the effect of temperature and stacking sequence alter the performance of entire panel system. The rises of temperature resulted in the decrements of the panel’s strength. This is due to the polymeric nature of this material. Additionally, the contact length also displays the effect on the performance of infill panel. Furthermore, the laminate stiffness can be modified by orientation of laminate, which can increase the infill panel strength. Hence, optimal performance of the entire panel system can be obtained by comparing different cases of stacking sequence.

Keywords: buckling resistance, GFRP infill panel, stacking sequence, temperature dependent

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Authors: Papon Thamvasupong, Kwanchanok Viravaidya-Pasuwat

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Osteoarthritis affects a lot of people worldwide. Local injection of glucosamine is one of the alternative treatment methods to replenish the natural lubrication of cartilage. However, multiple injections can potentially lead to possible bacterial infection. Therefore, a drug delivery system is desired to reduce the frequencies of injections. A hydrogel is one of the delivery systems that can control the release of drugs. Thermo-reversible hydrogels can be beneficial to the drug delivery system especially in the local injection route because this formulation can change from liquid to gel after getting into human body. Once the gel is in the body, it will slowly release the drug in a controlled manner. In this study, various formulations of Pluronic-based hydrogels were synthesized for the controlled release of glucosamine. One of the challenges of the Pluronic controlled release system is its fast dissolution rate. To overcome this problem, alginate and calcium sulfate (CaSO₄) were added to the polymer solution. The characteristics of the hydrogels were investigated including the gelation temperature, gelation time, hydrogel dissolution and glucosamine release mechanism. Finally, a mathematical model of glucosamine release from Pluronic-alginate-hyaluronic acid hydrogel was developed. Our results have shown that crosslinking Pluronic gel with alginate did not significantly extend the dissolution rate of the gel. Moreover, the gel dissolution profiles and the glucosamine release mechanisms were best described using the zeroth-order kinetic model, indicating that the release of glucosamine was primarily governed by the gel dissolution.

Keywords: controlled release, drug delivery system, glucosamine, pluronic, thermoreversible hydrogel

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Authors: Trabelsi Mohamed, Kharrat Mohamed, Dammak Maher

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Guide rings play an important role in the performance and durability of hydraulic actuating cylinders. In service, guide rings surfaces are subjected to friction and wear against steel counterface. A good mastery of these phenomena is required for the improvement of the energy safeguard and the durability of the actuating cylinder. Polytetrafluoroethylene (PTFE) polymer is extensively used in guide rings thanks to its low coefficient of friction, its good resistance to solvents as well as its high temperature stability. In this study, friction and wear behavior of two PTFE composites filled with bronze and bronze plus MoS2 were evaluated under oil-lubricated condition, aiming as guide rings for hydraulic actuating cylinder. Wear tests of the PTFE composite specimen sliding against steel ball were conducted using reciprocating linear tribometer. The wear mechanisms of the composites under the same sliding condition were discussed, based on Scanning Electron Microscopy examination of the worn composite surface and the optical micrographs of the steel counter surface. As for the results, comparative friction behaviors of the PTFE composites and lower friction coefficients were recorded under oil lubricated condition. The wear behavior was considerably improved to compare with this in dry sliding, while the oil adsorbed layer limited the transfer of the PTFE to the steel counter face during the sliding test.

Keywords: PTFE, composite, bronze, MoS2, friction, wear, oil-lubrication

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Authors: Betim Bahtiri, B. Arash, R. Rolfes

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Epoxy-based materials are frequently exposed to high-humidity environments in many engineering applications. As a result, their material properties would be degraded by water absorption. A full characterization of the material properties under hygrothermal conditions requires time- and cost-consuming experimental tests. To gain insights into the physics of diffusion mechanisms, atomistic simulations have been shown to be effective tools. Concerning the diffusion of water in polymers, spatial trajectories of water molecules are obtained from molecular dynamics (MD) simulations allowing the interpretation of diffusion pathways at the nanoscale in a polymer network. Conventional MD simulations of water diffusion in amorphous polymers lead to discrepancies at low temperatures due to the short timescales of the simulations. In the proposed model, this issue is solved by using a combined scheme of autonomous basin climbing (ABC) with kinetic Monte Carlo and reactive MD simulations to investigate the diffusivity of water molecules in epoxy resins across a wide range of temperatures. It is shown that the proposed simulation framework estimates kinetic properties of water diffusion in epoxy resins that are consistent with experimental observations and provide a predictive tool for investigating the diffusion of small molecules in other amorphous polymers.

Keywords: epoxy resins, water diffusion, autonomous basin climbing, kinetic Monte Carlo, reactive molecular dynamics

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Authors: Nataly De La Pava, Christian S. A. Silva-Torres, Arodí P. Favaris, José Maurício S. Bento

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The lady beetles Tenuisvalve notata and Cryptolaemus montrouzieri are important predators of mealybugs (Hemiptera: Pseudococcidae). Similar to the prey, these lady beetles produce wax filaments that cover their body during the larval stage. It has been hypothesized that lady beetle body wax chemical profiles are similar to their prey as i) a mechanism of camouflage and ii) conveying protection to the lady beetle larvae against aphid-tending predatory ants. In this study, we tested those hypotheses for the predators T. notata and C. montrouzieri and two mealybug prey species, Ferissia dasyrilii, and Planococcus citri. Next, we evaluated the influence of feeding on cuticular chemistry during predator development and identified possible metabolic costs associated with wax production. Cuticular wax samples were analyzed by GC-MS and GC-FID. Also, the metabolic cost linked to wax production was evaluated in the 4th instar larvae of the two predators when subjected to body wax removal from 0 to 4 times. Results showed that predator body wax profiles are not similar to the chemical profile of prey body wax. There was a metabolic cost associated with wax removal; predators (male and female) showed a significant reduction in adult body weight when the wax was removed. This suggests the reallocation of energy to wax replacement instead of growth. In addition, it was detected effects of wax removal on fecundity and egg viability. The results do not support the hypothesis that predators mimic the cuticular wax composition of prey as a means of camouflage.

Keywords: biological control, body wax, coccinellids, cuticular hydrocarbons, metabolism cost, reproduction

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Authors: Djamil Guettiche, Ahmed Mekki, Tighilt Fatma-Zohra, Rachid Mahmoud

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The aim of this study was to synthesize and characterize conducting polymer composites of polypyrrole and graphene, including pristine and surface-treated graphene (PPy/GO, PPy/rGO, and PPy/rGO-ArCOOH), for use as sensitive elements in a homemade chemiresistive module for on-line detection of nitrogen oxides vapors. The chemiresistive module was prepared, characterized, and evaluated for performance. Structural and morphological characterizations of the composite were carried out using FTIR, Raman spectroscopy, and XRD analyses. After exposure to NO and NO₂ gases in both static and dynamic modes, the sensitivity, selectivity, limit of detection, and response time of the sensor were determined at ambient temperature. The resulting sensor showed high sensitivity, selectivity, and reversibility, with a low limit of detection of 1 ppm. A composite of polypyrrole and graphene functionalized with aryl 4-carboxy benzene diazonium salt was synthesized and characterized using FTIR, scanning electron microscopy, transmission electron microscopy, UV-visible, and X-ray diffraction. The PPy-rGOArCOOH composite exhibited a good electrical resistance response to NO₂ at room temperature and showed enhanced NO₂-sensing properties compared to PPy-rGO thin films. The selectivity and stability of the NO₂ sensor based on the PPy/rGO-ArCOOH nanocomposite were also investigated.

Keywords: conducting polymers, surface treated graphene, diazonium salt, polypyrrole, Nitrogen oxide sensing

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Authors: Yeghnem Redha, Guerroudj Hicham Zakaria, Hanifi Hachemi Amar Lemiya, Meftah Sid Ahmed, Tounsi Abdelouahed, Adda Bedia El Abbas

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Creep deformation of concrete is often responsible for excessive deflection at service loads which can compromise the performance of elements within a structure. Although laboratory test may be undertaken to determine the deformation properties of concrete, these are time-consuming, often expensive and generally not a practical option. Therefore, relatively simple empirically design code models are relied to predict the creep strain. This paper reviews the accuracy of creep and shrinkage predictions of reinforced concrete (RC) shear walls structures strengthened with carbon fibre reinforced polymer (CFRP) sheets, which is characterized by a widthwise varying fibre volume fraction. This review is yielded by CEB-FIB MC90 model. The time-dependent behavior was investigated to analyze their static behavior. In the numerical formulation, the adherents and the adhesives are all modelled as shear wall elements, using the mixed finite element method. Several tests were used to dem¬onstrate the accuracy and effectiveness of the proposed method. Numerical results from the present analysis are presented to illustrate the significance of the time-dependency of the lateral displacements.

Keywords: RC shear walls strengthened, CFRP sheets, creep and shrinkage, CEB-FIP MC90 model, finite element method, static behavior

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Authors: Willi Zschiebsch, Alrik Dargel, Sebastian Spitzer, Philipp Johst, Robert Böhm, Niels Modler

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In this article, we investigate an approach that digitally links individual development process steps by using the drive shaft of an aircraft engine as a representative example of a fiber polymer composite. Such high-performance, lightweight composite structures have many adjustable parameters that influence the mechanical properties. Only a combination of optimal parameter values can lead to energy efficient lightweight structures. The development tools required for the Engineering Design Process (EDP) are often isolated solutions, and their compatibility with each other is limited. A digital framework is presented in this study, which allows individual specialised tools to be linked via the generated data in such a way that automated optimization across programs becomes possible. This is demonstrated using the example of linking geometry generation with numerical structural analysis. The proposed digital framework for automated design optimization demonstrates the feasibility of developing a complete digital approach to design optimization. The methodology shows promising potential for achieving optimal solutions in terms of mass, material utilization, eigenfrequency, and deformation under lateral load with less development effort. The development of such a framework is an important step towards promoting a more efficient design approach that can lead to stable and balanced results.

Keywords: digital linked process, composite, CFRP, multi-objective, EDP, NSGA-2, NSGA-3, TPE

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Authors: Donatella Cimini, Sergio D’ambrosio, Saba Sadiq, Chiara Schiraldi

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Chondroitin sulfate (CS), as well as modified CS, and unsulfated chondroitin, are largely applied in research today. CS is a linear glycosaminoglycan normally present in cartilage-rich tissues and bones in the form of proteoglycans decorated with sulfate groups in different positions. CS is used as an effective non-pharmacological alternative for the treatment of osteoarthritis, and other potential applications in the biomedical field are being investigated. Some bacteria, such as E. coli K4, produce a polysaccharide that is a precursor of CS (unsulfated chondroitin). This work focused on the construction of integrative E. coli K4 recombinant strains overexpressing genes (kfoA, kfoF, pgm and galU in different combinations) involved in the biosynthesis of the nucleotide sugars necessary for polysaccharide synthesis. Strain growth and polymer production were evaluated using renewable waste materials as substrates in shake flasks and small-scale batch fermentation processes. Results demonstrated the potential to replace pure sugars with cheaper medium components to establish environmentally sustainable and cost-effective production routes for potential industrial development. In fact, although excellent fermentation results have been described so far by employing strains that naturally produce chondroitin-like polysaccharides on semi-defined media, there is still the need to reduce manufacturing costs by providing a cost-effective biotechnological alternative to currently used animal-based extraction procedures.

Keywords: E. coli K4, chondroitin, microbial cell factories, glycosaminoglycans, renewable resources

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Authors: Asli Beyler Çi̇ği̇l, Memet Vezi̇r Kahraman

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Organic–inorganic hybrids have become an effective source of advanced materials because they combine the advantages of both the organic moiety such as flexibility, low dielectric constant, and processability, and inorganic moiety as rigidity, strength, durability, and thermal stability. By incorporating cross-linkable side chains, the hybrid materials can be made photosensitive and UV curable, which offers many advantages including low processing temperature, low equipment cost and compatibility. In this study, uv-curable organic-inorganic hybrid material, which was contained surface modified polyaniline particles (PANI), was prepared. PANI surface photografted with hydroxy ethyl methacrylate (HEMA) to produce hydroxyl groups. Hydroxyl functionalized PANI/HEMA was acrylated using isocyanato ethyl methacrylate (IEM) in order to improve the dispersion and interfacial interaction in composites. UV-curable formulation was prepared by mixing the surface modified PANI, polyethylene glycol diacrylate (PEGDA), trimethylolpropane triacrylate (TMPTA), hydrolized 3- methacryloxypropyltrimethoxysilane (hyd. MEMO) and photoinitiator. Chemical structure of nano-hybrid material was characterized by FTIR. FTIR spectra showed that the photografting of PANI was prepared successfully. Thermal properties of the nano-hybrid material were determined by thermogravimetric analysis (TGA). The morphology of the nano-hybrid material was performed by scanning electron microscopy (SEM).

Keywords: polyaniline, photograft, sol-gel, uv-curable polymer

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Authors: Justin Lee, Siraj Shaikh, Alice Chu MD

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Children with cerebral palsy (CP) commonly present with upper extremity impairment, affecting one or both extremities, and are classified using the Manual Ability Classification Scale (MACS). The MACS defines bimanual hand abilities for children ages 4-18 years in everyday tasks and is a gradient scale, with I being nearly normal and V requiring total assistance. Children with more severe upper extremity impairment (MACS III-V) are often underrepresented, and relatively few effective therapies have been identified for these patients. Current orthoses are static and are only meant to prevent the progression of contractures in these patients. Other limitations include cost, comfort, accessibility, and longevity of the orthoses. Taking advantage of advances in 3D printing technology, we have created a highly customizable upper extremity orthotic that can be produced at a low cost. Iterations in our design have resulted in an orthotic that is custom fit to the patient based on scans of their arm, made of rigid polymer when needed to provide support, flexible material where appropriate to allow for comfort, and designed with a mechanical pulley system to allow for some functional use of the arm while in the orthotic. Preliminary data has shown that our orthotic can be built at a fraction of the cost of current orthoses and provide clinically significant improvement in assisting hand assessment (AHA) and pediatric quality of life scores (PedsQL).

Keywords: upper extremity orthosis, upper extremity, orthosis, 3-D printing, cerebral palsy, occupational therapy, spasticity, customizable

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Authors: Javiera Poblete, Fernando Gajardo, Katherina Fernandez

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Graphene, and its derivatives such as graphene oxide (GO), are emerging nanoscopic materials, with interesting physical and chemical properties. From them, it is possible to develop three-dimensional macrostructures, such as aerogels, which are characterized by a low density, high porosity, and large surface area, having a promising structure for the development of materials. The use of GO as a precursor of these structures provides a wide variety of materials, which can be developed as a result of the functionalization of their oxygenated groups, with specific compounds such as polyethylene glycol (PEG). The synthesis of aerogels of GO-PEG for non-covalent interactions has not yet been widely reported, being of interest due to its feasible escalation and economic viability. Thus, this work aims to develop a non-covalently functionalized GO-PEG aerogels and characterize them physicochemically. In order to get this, the GO was synthesized from the modified hummers method and it was functionalized with the PEG by polymer-assisted GO gelation (crosslinker). The gelation was obtained for GO solutions (10 mg/mL) with the incorporation of PEG in different proportions by weight. The hydrogel resulting from the reaction was subsequently lyophilized, to obtain the respective aerogel. The material obtained was chemically characterized by analysis of Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray diffraction (XRD), and its morphology by scanning electron microscopy (SEM) images; as well as water absorption tests. The results obtained showed the formation of a non-covalent aerogel (FTIR), whose structure was highly porous (SEM) and with a water absorption values greater than 50% g/g. Thus, a methodology of synthesis for GO-PEG was developed and validated.

Keywords: aerogel, graphene oxide, polyethylene glycol, synthesis

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Authors: V.Barbakadze, L.Gogilashvili, L.Amiranashvili, M.Merlani, K.Mulkijanyan

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The high-molecular fractions from the several species of two genera (Symphytum and Anchusa) of Boraginaceae family Symphytum asperum, S. caucasicum, S. officinale, and Anchusa italica were isolated. According to IR, 13C and 1H NMR, 2D heteronuclear 1H/13C HSQC spectral data and 1D NOE experiment, the main structural element of these preparations was found to be a regularly substituted polyoxyethylene, namely poly[3-(3,4-dihydroxyenyl)glyceric acid] (PDPGA) or poly[oxy-1-carboxy-2-(3,4-dihydroxyphenyl)ethylene]. Such caffeic acid-derived biopolymer to our knowledge has not been known and has been identified for the first time. This compound represents a new class of natural polyethers with a residue of 3-(3,4-dihydroxyphenyl)glyceric acid as the repeating unit. Most of the carboxylic groups of PDPGA from A. italica unlike the polymer of S. asperum, S. caucasicum, and S. officinale are methylated. The 2D DOSY experiment gave the similar diffusion coefficient for the methylated and non-methylated signals of A. italica PDPGA. Both sets of signals fell in the same horizontal. This would imply a similar molecular weight for methylated and non-methylated polymers. This was further evidenced by graphic representations of the intensity decay of the 1H signals of aromatic H-2″ and H-1 at δ 7.16 and 5.24 and that of the methoxy group at δ 3.85. These three signals essentially showed the same curve shape. According to results of in vitro and in vivo experiments PDPGA of S.asperum and S.caucasicum could be considered as potential anti-inflammatory, wound healing and anti-cancer therapeutic agent.

Keywords: caffeic acid-derived polyether, poly[3-(3, 4-dihydroxyphenyl)glyceric acid], poly[oxy-1-carboxy-2-(3, 4-dihydroxyphenyl)ethylene], symphytum, anchusa

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Authors: Mustafa Abu Ghalia, Mohammed Seddik

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The design and development of a new class of biomaterial has gained particular interest in producing polymer scaffold for biomedical applications. Improving mechanical properties, biological and controlling pores scaffold are important factors to provide appropriate biomaterial for implement in soft tissue repair and regeneration. In this study, poly-ε-caprolactone (PCL) /polyethylene glycol (PEG) copolymer (80/20) incorporated with CNF scaffolds were made employing solvent casting and particulate leaching methods. Four mass percentages of CNF (1, 2.5, 5, and 10 wt.%) were integrated into the copolymer through a silane coupling agent. Mechanical properties were determined using Tensile Tester data acquisition to investigate the effect of porosity, pore size, and CNF contents. Tensile strength obtained for PCL/PEG- 5 wt.% CNF was 16 MPa, which drastically decreased after creating a porous structure to 7.1 MPa. The optimum parameters of the results were found to be 5 wt.% for CNF, 240 μm for pore size, and 83% for porosity. Scanning electron microscopy (SEM) micrograph reveals that consistent pore size and regular pore shape were accomplished after the addition of CNF-5 wt. % into PCL/PEG. The results of mass loss of PCL/PEG reinforced-CNF 1% have clearly enhanced to double values compared with PCL/PEG copolymer and three times with PCL/PEG scaffold-CNF 1%. In addition, all PCL/PEG reinforced and scaffold- CNF were partially disintegrated under composting conditions confirming their biodegradable behavior. This also provides a possible solution for the end life of these biomaterials.

Keywords: PCL/PEG, cellulose nanofibers, tissue engineering, biodegradation, compost polymers

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Authors: Sarra Boughaba

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The α-aminophosphonates have received considerable attention in organic and medicinal chemistry because of their structural resemblance with α-amino acids. They are used as antitumor agents, anti-inflammatory and antibiotics. As a result, a number of procedures have been developed for their synthesis. However, many of these methods suffer from some disadvantages such as long reaction times, environmental pollution caused by utilization of organic solvents, and expensive catalyst. On the other hand, thiazole components, particularly 2-aminothiazole is an important class of heterocyclic compounds. They appear in the structure of natural products and biologically actives compounds, thiamine (vitamin-B), and some antibiotics drugs (penicillin, micrococcin). In the past few years, heteropolyacids have received great attention as environmentally benign catalysts for organic synthetic processes, they possess unique physicochemical properties, such as super-acidity, high thermal and chemical stability, ability to accept and release electrons and high proton mobility, and the possibility of varying their acidity and oxidizing potential. In this study, an efficient and eco-friendly process has been developed for the synthesis of α-aminophosphonates containing aminothiazole moiety via Kabachnik-Field reaction catalyzed by H₆P₂W₁₈O₆₂.14H₂O as reusable catalyst, by condensation of aromatic aldehydes, 2-aminothiazole and triethylphosphite under free conditions. The X-ray crystallographic data of obtained compounds were provided. The main advantages of our protocol include the absence of solvent in the reaction, easy work-up, short reaction time, atom-economy and reusability of catalyst without significant loss of its activity.

Keywords: aminophosphonates, green synthesis, H₆P₂W₁₈O₆₂.14H₂O catalyst, x-ray study

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Authors: Nioushasadat Haji Seyed Javadi, Ailar Hajimohammadi, Nasser Khalili

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Currently, the recycling of plastic wastes has been the subject of much research attention, especially in pavement constructions, where virgin polymers can be replaced by recycled plastics for asphalt binder modification. Among the plastic types, recycled linear low-density polyethylene (RLLDPE) has been one of the common and largely available plastics for bitumen modification. However, it is important to note that during the recycling process, LLDPE can easily be contaminated with other plastic types, especially with low-density polyethylene (LDPE), high-density polyethylene (HDPE), and polypropylene (PP). The cross-contamination of LLDPE with other plastics lowers its quality and, consequently, can affect the asphalt modification process. This study aims to assess the effect of LLDPE cross-contamination on bitumen modification. To do so, samples of bitumen modified with LLDPE and blends of LLDPE with LDPE, HDPE, and PP were prepared and compared through physical and rheological evaluations. The experimental tests, including softening point, penetration, viscosity at 135 °C, and dynamic shear rheometer, were conducted. The results indicated that the effect of cross-contamination on softening point and rutting resistance was negligible. On the other side, penetration and viscosity were highly impacted. The results also showed that among contamination of LLDPE with the other plastic types, PP had the highest influence in comparison with HDPE and LDPE on changing the properties of the LLDPE- modified bitumen.

Keywords: recycled polyethylene, polymer cross-contamination, waste plastic, bitumen, rutting resistance

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Authors: Itti Bist, Snehasis Bhakta, Di Jiang, Tia E. Keyes, Aaron Martin, Robert J. Forster, James F. Rusling

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DNA damage from metabolites of lipophilic drugs and pollutants, generated by enzymes, represents a major toxicity pathway in humans. These metabolites can react with DNA to form either 8-oxo-7,8-dihydro-2-deoxyguanosine (8-oxodG), which is the oxidative product of DNA or covalent DNA adducts, both of which are genotoxic and hence considered important biomarkers to detect cancer in humans. Therefore, detecting reactions of metabolites with DNA is an effective approach for the safety assessment of new chemicals and drugs. Here we describe a novel electrochemiluminescent (ECL) sensor array which can detect DNA oxidation and chemical DNA damage in a single array, facilitating a more accurate diagnostic tool for genotoxicity screening. Layer-by-layer assembly of DNA and enzyme are assembled on the pyrolytic graphite array which is housed in a microfluidic device for sequential detection of two type of the DNA damages. Multiple enzyme reactions are run on test compounds using the array, generating toxic metabolites in situ. These metabolites react with DNA in the films to cause DNA oxidation and chemical DNA damage which are detected by ECL generating osmium compound and ruthenium polymer, respectively. The method is further validated by the formation of 8-oxodG and DNA adduct using similar films of DNA/enzyme on magnetic bead biocolloid reactors, hydrolyzing the DNA, and analyzing by liquid chromatography-mass spectrometry (LC-MS). Hence, this combined DNA/enzyme array/LC-MS approach can efficiently explore metabolic genotoxic pathways for drugs and environmental chemicals.

Keywords: biosensor, electrochemiluminescence, DNA damage, microfluidic array

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Authors: Ozlem Temiz Arpaci, Meryem Tasci, Hakan Goker

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Benzimidazole, a structural isostere of indol and purine nuclei that can interact with biopolymers, can be identified as master key. So that benzimidazole compounds are important fragments in medicinal chemistry because of their wide range of biological activities including antimicrobial activity. We planned to synthesize some benzimidazole compounds for developing new antimicrobial drug candidates. In this study, we put some heterocyclic rings on second position and an amidine group on the fifth position of benzimidazole ring and synthesized them using a multiple step procedure. For the synthesis of the compounds, as the first step, 4-chloro-3-nitrobenzonitrile was reacted with cyclohexylamine in dimethyl formamide. Imidate esters (compound 2) were then prepared with absolute ethanol saturated with dry HCl gas. These imidate esters which were not too stable were converted to compound 3 by passing ammonia gas through ethanol. At the Pd / C catalyst, the nitro group is reduced to the amine group (compound 4). Finally, various aldehyde derivatives were reacted with sodium metabisulfite addition products to give compound 5-20. Melting points were determined on a Buchi B-540 melting point apparatus in open capillary tubes and are uncorrected. Elemental analyses were done a Leco CHNS 932 elemental analyzer. 1H-NMR and 13C-NMR spectra were recorded on a Varian Mercury 400 MHz spectrometer using DMSO-d6. Mass spectra were acquired on a Waters Micromass ZQ using the ESI(+) method. The structures of them were supported by spectral data. The 1H-NMR, 13C NMR and mass spectra and elemental analysis results agree with those of the proposed structures. Antimicrobial activity studies of the synthesized compounds are under the investigation.

Keywords: benzimidazoles, synthesis, structure elucidation, antimicrobial

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Authors: J. Pazourek, K. Šmejkal, P. Kollár, J. Rajchard, J. Šinko, Z. Balounová, E. Vlková, H. Salmonová

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Pectinatella magnifica (Leidy, 1851) is an invasive freshwater animal that lives in colonies. A colony of Pectinatella magnifica (a gelatinous blob) can be up to several feet in diameter large and under favorable conditions it exhibits an extreme growth rate. Recently European countries around rivers of Elbe, Oder, Danube, Rhine and Vltava have confirmed invasion of Pectinatella magnifica, including freshwater reservoirs in South Bohemia (Czech Republic). Our project (Czech Science Foundation, GAČR P503/12/0337) is focused onto biology and chemistry of Pectinatella magnifica. We monitor the organism occurrence in selected South Bohemia ponds and sandpits during the last years, collecting information about physical properties of surrounding water, and sampling the colonies for various analyses (classification, maps of secondary metabolites, toxicity tests). Because the gelatinous matrix is during the colony lifetime also a host for algae, bacteria and cyanobacteria (co-habitants), in this contribution, we also applied a high performance liquid chromatography (HPLC) method for determination of potentially present cyanobacterial toxins (microcystin-LR, microcystin-RR, nodularin). Results from the last 3-year monitoring show that these toxins are under limit of detection (LOD), so that they do not represent a danger yet. The final goal of our study is to assess toxicity risks related to fresh water resources invaded by Pectinatella magnifica, and to understand the process of invasion, which can enable to control it.

Keywords: cyanobacteria, fresh water resources, Pectinatella magnifica invasion, toxicity monitoring

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Authors: Lakshmi Sirisha Kotikalapudi

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Atenolol, the widely used antihypertensive drug is ionisable and degrades in the acidic environment of the GIT lessening the bioavailability. Transdermal route may be selected as an alternative to enhance the bioavailability. Half-life of the drug is 6-7 hours suggesting the requirement of prolonged release of the drug. The present work of transdermal niosomal gel aims to extend release of the drug and increase the bioavailability. Ethanol injection method was used for the preparation of niosomes using span-60 and cholesterol at different molar ratios following central composite design. The prepared niosomes were characterized for size, zeta-potential, entrapment efficiency, drug content and in-vitro drug release. Optimized formulation was selected by statistically analyzing the results obtained using the software Stat-Ease Design Expert. The optimized formulation also showed high drug retention inside the vesicles over a period of three months at a temperature of 4 °C indicating stability. Niosomes separated as a pellet were dried and incorporated into the hydrogel prepared using chitosan a natural polymer as a gelling agent. The effect of various chemical permeation enhancers was also studied over the gel formulations. The prepared formulations were characterized for viscosity, pH, drug release using Franz diffusion cells, and skin irritation test as well as in-vivo pharmacological activities. Atenolol niosomal gel preparations showed the prolonged release of the drug and pronounced antihypertensive activity indicating the suitability of niosomal gel for topical and systemic delivery of atenolol.

Keywords: atenolol, chitosan, niosomes, transdermal

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Authors: Anjana Jain, S. Jayanth Kumar

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

Keywords: dielectric Properties, PANI, PVDF, smart materials

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Authors: Chen-En Lin, Lih-Rou Rau, Jiunn-Woei Liaw, Shiao-Wen Tsai

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The unique optical properties of plasmon resonance metallic particles have attracted considerable applications in the fields of physics, chemistry and biology. Metal-Enhanced Fluorescence (MEF) effect is one of the useful applications. MEF effect stated that fluorescence intensity can be quenched or be enhanced depending on the distance between fluorophores and the metal nanoparticles. Silver nanoparticles have used widely in antibacterial studies. However, the major limitation for silver nanoparticles (AgNPs) in biomedical application is well-known cytotoxicity on cells. There were numerous literatures have been devoted to overcome the disadvantage. The aim of the study is to evaluate the cytotoxicity and biocompatibility of silica coated AgNPs against NIH-3T3 cells. The results were shown that NIH-3T3 cells started to detach, shrink, become rounded and finally be irregular in shape after 24 h of exposure at 10 µg/ml AgNPs. Besides, compared with untreated cells, the cell viability significantly decreased to 60% and 40% which were exposed to 10 µg/ml and 20 µg/ml AgNPs respectively. The result was consistent with previously reported findings that AgNPs induced cytotoxicity was concentration dependent. However, the morphology and cell viability of cells appeared similar to the control group when exposed to 20 µg/ml of silica coated AgNPs. We further utilized the dark-field hyperspectral imaging system to analysis the optical properties of the intracellular nanoparticles. The image displayed that the red shift of the surface plasmonic resonances band of the enclosed AgNPs further confirms the agglomerate of the AgNPs rather than their distribution in cytoplasm. In conclusion, the study demonstrated the silica coated of AgNPs showed well biocompatibility and significant lower cytotoxicity compared with bare AgNPs.

Keywords: silver nanoparticles, silica, cell viability, morphology

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Authors: Temnov D., Volgina E., Gerasimov D.

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Relaxation processes in polyvinylidene fluoride (PVDF) films were studied by the method of thermally stimulated fractional polarization currents (TSTF). The films were obtained by extrusion of a polymer melt followed by isometric annealing. PVDF granules of the Kynar-720 brand (Atofina Chemicals, USA) with a molecular weight of Mw=190,000 g•mol-1 were used for the manufacture of films. The annealing temperature was varied in the range from 120 °C to 170 °C in increments of 10 °C. The dependences of the degree of crystallinity of films (χ) and the intensity of thermally stimulated depolarization currents on the annealing temperature (Toc) are investigated. The TSTF spectra were obtained at the TSC II facility (Setaram, France). Measurements were carried out in a helium atmosphere, and the values of currents were determined by a Keithley electrometer. The annealed PVDF films were polarized at an electric field strength of 100 V/mm at a temperature of 31°C, after which they were cooled to 26°C, at which they were kept for 1 minute. During depolarization, the external field was removed, and the short-circuit sample was cooled to 0°C. The thermally stimulated short-circuit current was recorded during linear heating. Relaxation processes in PVDF films were studied in the temperature range from 0 – 70 °C. It is shown that the intensity curve of the peaks of TST FP has a course that is the reverse of the dependence of the degree of crystallinity on the annealing temperature. This allows us to conclude that the relaxation processes occurring in PVDF in the 35°C region are associated with the amorphous part of the structure of PVDF films between the layers of the spherulite crystalline phase.

Keywords: molecular and supramolecular structure, thermally stimulated currents, polyvinylidene fluoride films, relaxation processes

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Authors: D. Karibasavaraja, Ramesh M.R., Sufiyan Ahmed, Noyonika M.R., Sameeksha A. V., Mamatha J., Samiksha S. Urs

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This research paper gives an overview of the experimental analysis of natural fibers with polymer composite. The whole world is concerned about conserving the environment. Henceforth, the demand for natural and decomposable materials is increasing. The application of natural fibers is widely used in aerospace for manufacturing aircraft bodies, and ship construction in navy fields. Based on the literature review, researchers and scientists are replacing synthetic fibers with natural fibers. The selection of these fibers mainly depends on lightweight, easily available, and economical and has its own physical and chemical properties and many other properties that make them a fine quality fiber. The pineapple fiber has desirable properties of good mechanical strength, high cellulose content, and fiber length. Hybrid composite was prepared using different proportions of pineapple fiber and banana fiber, and their ratios were varied in 90% polypropylene mixed with 5% banana fiber and 5% pineapple fiber, 85% polypropylene mixed with 7.5% banana fiber and 7.5% pineapple fiber and 80% polypropylene mixed with 10% banana fiber and 10% pineapple fiber. By impact experimental analysis, we concluded that the combination of 90% polypropylene and 5% banana fiber and 5% pineapple fiber exhibits a higher toughness value with mechanical strength. We also conducted scanning electron microscopy (SEM) analysis which showed better fiber orientation bonding between the banana and pineapple fibers with polypropylene composites. The main aim of the present research is to evaluate the properties of pineapple fiber and banana fiber reinforced with hybrid polypropylene composites.

Keywords: toughness, fracture, impact strength, banana fibers, pineapple fibers, tensile strength, SEM analysis

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Authors: Layla El Gaini, Majdouline Belaqziz, Meriem Outaki, Mariam Minhaj

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In this study, it introduce and validate a high-performance liquid chromatography method with diode-array detection (HPLC-DAD) specifically designed for the accurate quantification of caffeic acid in phenolic extracts obtained from olive mill wastewater. The separation process of caffeic acid was effectively achieved through the use of an Acclaim Polar Advantage column (5µm, 250x4.6mm). A meticulous multi-step gradient mobile phase was employed, comprising water acidified with phosphoric acid (pH 2.3) and acetonitrile, to ensure optimal separation. The diode-array detection was adeptly conducted within the UV–VIS spectrum, spanning a range of 200–800 nm, which facilitated precise analytical results. The method underwent comprehensive validation, addressing several essential analytical parameters, including specificity, repeatability, linearity, as well as the limits of detection and quantification, alongside measurement uncertainty. The generated linear standard curves displayed high correlation coefficients, underscoring the method's efficacy and consistency. This validated approach is not only robust but also demonstrates exceptional reliability for the focused analysis of caffeic acid within the intricate matrices of wastewater, thus offering significant potential for applications in environmental and analytical chemistry.

Keywords: high-performance liquid chromatography (HPLC-DAD), caffeic acid analysis, olive mill wastewater phenolics, analytical method validation

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Authors: Mehrdad Gholami, Shima Behkami, Sharifuddin B. Md. Zain, Firdaus A. B. Kamaruddin

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Starting from the first application of a microwave oven for sample preparation in 1975 for the purpose of wet ashing of biological samples using a domestic microwave oven, many microwave-assisted dissolution vessels have been developed. The advanced vessels are armed with special safety valve that release the excess of pressure while the vessels are in critical conditions due to applying high power of microwave. Nevertheless, this releasing of pressure may cause lose of volatile elements. In this study Teflon bottles are designed with relatively thicker wall compared to commercial ones and a silicone based polymer was used to prepare an O-ring which plays the role of safety valve. In this design, eight vessels are located in an ABS holder to keep them stable and safe. The advantage of these vessels is that they need only 2 mL of HNO3 and 1mL H2O2 to digest different environmental samples, namely, sludge, apple leave, peach leave, spinach leave and tomato leave. In order to investigate the performance of this design an ICP-MS instrument was applied for multi elemental analysis of 20 elements on the SRM of above environmental samples both using this design and a commercial microwave digestion design. Very comparable recoveries were obtained from this simple design with the commercial one. Considering the price of ultrapure chemicals and the amount of them which normally is about 8-10 mL, these simple vessels with the procedures that will be discussed in detail are very cost effective and very suitable for environmental studies.

Keywords: inductively coupled plasma mass spectroscopy (ICP-MS), PTFE vessels, Teflon bombs, microwave digestion, trace element

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Authors: Timo Avikainen, Tuukka Verho

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The use of natural fibers as reinforcements is growing increasingly in polymers which are involved in e.g. structural, vibration, and acoustic applications. The use of bio composites is being investigated as lightweight materials with specific properties like the ability to dissipate vibration energy and positive environmental profile and are thus considered as potential replacements for synthetic composites. The macro-level mechanical properties of the biocomposite material depend on several parameters in the detailed architecture and morphology of the reinforcing fiber structure. The polymer matrix phase is often applied to remain the fiber structure in touch. A big role in the packaging details of the fibers is related to the used manufacturing processes like extrusion, injection molding and treatments. There are typically big variances in the detailed parameters of the microstructure fibers. The study addressed the question of how the multiscale simulation methodology works in bio composites with short pulp fibers. The target is to see how the vibro – acoustic performance of thin–walled panels can be controlled by the detailed characteristics of the fiber material. Panels can be used in sound-producing speakers or sound insulation applications. The multiscale analysis chain is tested starting from the microstructural level and continuing via macrostructural material parameters to the product component part/assembly levels. Another application is the dynamic impact type of loading, exposing the material to the crack type damages that is in this study modeled as the Charpy impact tests.

Keywords: bio composite, pulp fiber, vibration, acoustics, impact, FEM

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Authors: Asmaa M. Fahim

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In this elucidation, we synthesized different heterocyclic compounds attached to Benzene sulfonamide moiety via (E)-N-(4-(3-(4-bromophenyl)acryloyl)phenyl)-4-methyl benzene sulfonamide which is obtained from Nucleophilic substitution reaction between 4-methylbenzene sulfonyl chloride and 1-(4-aminophenyl)ethan-1-one in pyridine to get N-(4-acetyl phenyl)-4-methyl benzenesulfonamide which reacted 4-bromobenzal dehyde undergoes aldol condensation in NaOH to afford the corresponding chalchone 4. Moreover, the reactivity of chalchone 4 showed several active methylene derivatives utilized the pressurized microwave irradiation as a green energy resource. Chalcone 4 was allowed to react with ethyl cyanoacetate and acetylacetone, respectively, at 70 °C with pressure under microwave reaction condition to afford the 5-cyano-6-oxo-1,2,5,6-tetrahydropyridin-2-yl)-4-methylbenzenesulfonamide 6 and N-(4'-acetyl-4''-bromo-5'-oxo-2',3',4',5'-tetrahydro-[1,1':3',1''-terphenyl]-4-yl)-4-methylbenzenesulfonamide 8 derivatives. Moreover, the reactivity of this sulphonamide chalchone with NH2NH2 in EtOH and acetic acid, which gave 2,5-dihydro-1H-imidazol-4-yl)-4-methyl benzenesulfonamide, 1H-pyrazol-3-yl)-4-methyl and reactivity with NH2OH.HCl gave isoxazol-3-yl)-4-methylbenzenesulfonamide derivatives. The synthesized compounds were screened for their ADME properties and directed to antitumor activity on HepG2 hepatocellular carcinoma and MCF-7 breast cancer and exhibited excellent behavior against standard drugs; these results were confirmed through molecular simulations with different proteins. Additionally, the Density Functional Theory analysis of optimized structures investigated their physical descriptors, FMO, ESP and MEP, which correlated with biological evaluation.

Keywords: synthesis, green chemistry, antitumor activity, DFT study

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Authors: Lia Gventsadze, Elguja Kutelia, David Gventsadze

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The purpose of the article is to show the possibility for the development of a new generation, eco-friendly (asbestos free) nano-porous friction materials on the basis of Georgian raw materials, along with the determination of technological parameters for their production, as well as the optimization of tribological properties and the investigation of structural aspects of wear peculiarities of elaborated materials using the scanning electron microscopy (SEM) and Auger electron spectroscopy (AES) methods. The study investigated the tribological properties of the polymer friction materials on the basis of the phenol-formaldehyde resin using the porous diatomite filler modified by silane with the aim to improve the thermal stability, while the composition was modified by iron phosphate, technical carbon and basalt fibre. As a result of testing the stable values of friction factor (0.3-0,45) were reached, both in dry and wet friction conditions, the friction working parameters (friction factor and wear stability) remained stable up to 500 OC temperatures, the wear stability of gray cast-iron disk increased 3-4 times, the soundless operation of materials without squeaking were achieved. Herewith it was proved that small amount of ingredients (5-6) are enough to compose the nano-porous friction materials. The study explains the mechanism of the action of nano-porous composition base brake lining materials and its tribological efficiency on the basis of the triple phase model of the tribo-pair.

Keywords: brake lining, friction coefficient, wear, nanoporous composite, phenolic resin

Procedia PDF Downloads 393