Search results for: hyperspectral scanning

Authors: José M. Liñeira Del Río, Ramón Rial, Khodor Nasser, María J.G. Guimarey

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The need to develop new lubricants that offer better anti-friction and anti-wear performance in internal combustion vehicles is one of the great challenges of lubrication in the automotive field. The addition of nanoparticles has emerged as a possible solution and, combined with the lubricating power of ionic liquids, may become one of the alternatives to reduce friction losses and wear of the contact surfaces in the conditions to which tribo-pairs are subjected, especially in the contact of the piston rings and the cylinder liner surface. In this study, the improvement in SAE 10W-40 engine oil tribological performance after the addition of magnesium oxide (MgO) nanoadditives and two different phosphonium-based ionic liquids (ILs) was investigated. The nanoparticle characterization was performed by means of transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The tribological properties, friction coefficients and wear parameters of the formulated oil modified with 0.01 wt.% MgO and 1 wt.% ILs compared with the neat 10W-40 oil were performed and analyzed using a ball-on-three-pins tribometer and a 3D optical profilometer, respectively. Further analysis on the worn surface was carried out by Raman spectroscopy and SEM microscopy, illustrating the formation of the protective IL and MgO tribo-films as hybrid additives. In friction tests with sliding steel-steel tribo-pairs, IL3-based hybrid nanolubricant decreased the friction coefficient and wear volume by 7% and 59%, respectively, in comparison with the neat SAE 10W-40, while the one based on IL1 only achieved a reduction of these parameters by 6% and 39%, respectively. Thus, the tribological characterization also revealed that the MgO and IL3 addition has a positive synergy over the commercial lubricant, adequately meeting the requirements for their use in internal combustion engines. In summary, this study has shown that the addition of ionic liquids to MgO nanoparticles can improve the stability and lubrication behavior of MgO nanolubricant and encourages more investigations on using nanoparticle additives with green solvents such as ionic liquids to protect the environment as well as prolong the lifetime of machinery. The improvement in the lubricant properties was attributed to the following wear mechanisms: the formation of a protective tribo-film and the ability of nanoparticles to fill out valleys between asperities, thereby effectively smoothing out the shearing surfaces.

Keywords: lubricant, nanoparticles, phosphonium-based ionic liquids, tribology

Procedia PDF Downloads 82

Authors: Mohamed Rehan, Gamil E. Ibrahim, Mohamed S. Abdel-Aziz, Shaimaa R. Ibrahim, Tawfik A. Khattab

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The utilization of natural products in finishing textiles toward multifunctional applications without side effects is an extremely motivating goal. Hibiscus sabdariffa usually has been used for many traditional medicine applications. To develop an additional use for Hibiscus sabdariffa, an extraction of bioactive compounds from Hibiscus sabdariffa followed by finishing on cellulosic fibers was designed to cleaner production of the value-added textiles fibers with multifunctional applications. The objective of this study is to explore, identify, and evaluate the bioactive compound extracted from Hibiscus sabdariffa by different solvent via ultrasonic technique as a potential eco-friendly agent for multifunctional cellulosic fabrics via two approaches. In the first approach, Hibiscus sabdariffa extract was used as a source of sustainable eco-friendly for simultaneous coloration and multi-finishing of cotton fabrics via in situ incorporations of nanoparticles (silver and metal oxide). In the second approach, the micro-capsulation of Hibiscus sabdariffa extracts was followed by coating onto cotton gauze to introduce multifunctional healthcare applications. The effect of the solvent type was accelerated by ultrasonic on the phytochemical, antioxidant, and volatile compounds of Hibiscus sabdariffa. The surface morphology and elemental content of the treated fabrics were explored using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), and energy-dispersive X-ray spectroscopy (EDX). The multifunctional properties of treated fabrics, including coloration, sensor properties and protective properties against pathogenic microorganisms and UV radiation as well as wound healing property were evaluated. The results showed that the water, as well as ethanol/water, was selected as a solvent for the extraction of natural compounds from Hibiscus Sabdariffa with high in extract yield, total phenolic contents, flavonoid contents, and antioxidant activity. These natural compounds were utilized to enhance cellulosic fibers functionalization by imparting faint/dark red color, antimicrobial against different organisms, and antioxidants as well as UV protection properties. The encapsulation of Hibiscus Sabdariffa extracts, as well as wound healing, is under consideration and evaluation. As a result, the current study presents a sustainable and eco-friendly approach to design cellulosic fabrics for multifunctional medical and healthcare applications.

Keywords: cellulosic fibers, Hibiscus sabdariffa extract, multifunctional application, nanoparticles

Procedia PDF Downloads 146

Authors: Abdulqader Alkhouzaam, Hazim Qiblawey, Majeda Khraisheh

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Membrane treatment for desalination and wastewater treatment is one of the promising solutions to affordable clean water. It is a developing technology throughout the world and considered as the most effective and economical method available. However, the limitations of membranes’ mechanical and chemical properties restrict their industrial applications. Hence, developing novel membranes was the focus of most studies in the water treatment and desalination sector to find new materials that can improve the separation efficiency while reducing membrane fouling, which is the most important challenge in this field. Graphene oxide (GO) is one of the materials that have been recently investigated in the membrane water treatment sector. In this work, ultrafiltration polysulfone (PSF) membranes with high antifouling properties were synthesized by incorporating different loadings of GO. High-oxidation degree GO had been synthesized using a modified Hummers' method. The synthesized GO was characterized using different analytical techniques including elemental analysis, Fourier transform infrared spectroscopy - universal attenuated total reflectance sensor (FTIR-UATR), Raman spectroscopy, and CHNSO elemental analysis. CHNSO analysis showed a high oxidation degree of GO represented by its oxygen content (50 wt.%). Then, ultrafiltration PSF membranes incorporating GO were fabricated using the phase inversion technique. The prepared membranes were characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM) and showed a clear effect of GO on PSF physical structure and morphology. The water contact angle of the membranes was measured and showed better hydrophilicity of GO membranes compared to pure PSF caused by the hydrophilic nature of GO. Separation properties of the prepared membranes were investigated using a cross-flow membrane system. Antifouling properties were studied using bovine serum albumin (BSA) and humic acid (HA) as model foulants. It has been found that GO-based membranes exhibit higher antifouling properties compared to pure PSF. When using BSA, the flux recovery ratio (FRR %) increased from 65.4 ± 0.9 % for pure PSF to 84.0 ± 1.0 % with a loading of 0.05 wt.% GO in PSF. When using HA as model foulant, FRR increased from 87.8 ± 0.6 % to 93.1 ± 1.1 % with 0.02 wt.% of GO in PSF. The pure water permeability (PWP) decreased with loadings of GO from 181.7 L.m⁻².h⁻¹.bar⁻¹ of pure PSF to 181.1, and 157.6 L.m⁻².h⁻¹.bar⁻¹ with 0.02 and 0.05 wt.% GO respectively. It can be concluded from the obtained results that incorporating low loading of GO could enhance the antifouling properties of PSF hence improving its lifetime and reuse.

Keywords: antifouling properties, GO based membranes, hydrophilicity, polysulfone, ultrafiltration

Procedia PDF Downloads 143

Authors: Javad Saeidaskari, Mohammad Hassan Baziar

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Soil structures have been frequently damaged during piping, earthquake and other types of failures. As far as adverse circumstances were developed subsequent to piping or other similar failure types, hydraulic parameters of soil such as hydraulic conductivity should be considered. As a result, acquiring an approach to diminish soil permeability is inevitable. There are many ground improvement methods to reduce seepage, which are classified under soil treatment and stabilization methods. Recently, one of the soil improvement methods is known as nanogeotechnology. This study aims to investigate the influence of Cloisite 30B nanoclay on permeability of compacted clayey sand soils. The samples are prepared by mixing two soil types, including Kaolin clay and Firouzkooh sand, in 1:9 and 1:5 clay:sand (by mass) proportions. In experimental procedure, initially, the optimum water content and maximum dry unit weight of each samples were obtained for compaction. Then, series of permeability tests were conducted by triaxial apparatus on prepared specimens with identical relative density of 95% of maximum dry density and water content of 1% wet of optimum for different weight percentages of nanoclay (1% to 4%). Therefore, in this paper, the effect of time on treated specimen was appraised, as well as two approaches of manual mixing and ball milling were compared to reveal the importance of dispersion issue. The results show that adding nanoclay up to 3%, as its optimum content, causes notable reduction in permeability (1.60e-03 to 5.51e-05 cm/s and 3.32e-04 to 8.44e-07 cm/s in samples with 1:9 and 1:5 mixture proportions, respectively). The hydraulic conductivity of treated clayey sand (1:5 mixture proportion with 3% nanoclay) decreases gradually from 8.44e-07 to 3.00e-07 cm/s within 90 days and then tends to be consistent. The influence of mixing method on permeability results shows that the utilization of ball mill mixing effectively leads to lower values than those of manual mixing, in other words, by adding 3% nanoclay, hydraulic conductivity of specimen declines from 8.44e-07 to 2.00e-07 cm/s. In order to evaluate the interaction between soil particles and, to ensure proper dispersion of nanoparticles through clayey sand mixture, they were magnified by means of scanning electron microscope (SEM). In conclusion, the nanoclay particles in vicinity of moisture can cause soil stabilization to prevent water penetration, which eventually result in lower usage of clay and operation costs.

Keywords: nanoclay, cloisite 30b, clayey sand, hydraulic conductivity

Procedia PDF Downloads 349

Authors: Ahmed F. Ghanem, Marwa I. Wahba, Asmaa N. El-Dein, Mohamed A. EL-Raey, Ghada E.A. Awad

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Numerous attempts are being performed in order to formulate suitable packaging materials for meat products. However, to the best of our knowledge, the incorporation of free hibiscus extract or its microcapsules in the pure polyvinyl alcohol (PVA) matrix as packaging materials for meats is seldom reported. Therefore, this study aims at protection of the aqueous crude extract of hibiscus flowers utilizing spry drying encapsulation technique. Fourier transform infrared (FTIR), scanning electron microscope (SEM), and zetasizer results confirmed the successful formation of assembled capsules via strong interactions, spherical rough microparticles, and ~ 235 nm of particle size, respectively. Also, the obtained microcapsules enjoy high thermal stability, unlike the free extract. Then, the obtained spray-dried particles were incorporated into the casting solution of the pure PVA film with a concentration 10 wt. %. The segregated free-standing composite films were investigated, compared to the neat matrix, with several characterization techniques such as FTIR, SEM, thermal gravimetric analysis (TGA), mechanical tester, contact angle, water vapor permeability, and oxygen transmission. The results demonstrated variations in the physicochemical properties of the PVA film after the inclusion of the free and the extract microcapsules. Moreover, biological studies emphasized the biocidal potential of the hybrid films against microorganisms contaminating the meat. Specifically, the microcapsules imparted not only antimicrobial but also antioxidant activities to PVA. Application of the prepared films on the real meat samples displayed low bacterial growth with a slight increase in the pH over the storage time up to 10 days at 4 oC which further proved the meat safety. Moreover, the colors of the films did not significantly changed except after 21 days indicating the spoilage of the meat samples. No doubt, the dual-functional of prepared composite films pave the way towards combined active/smart food packaging applications. This would play a vital role in the food hygiene, including also quality control and assurance.

Keywords: PVA, hibiscus, extraction, encapsulation, active packaging, smart and intelligent packaging, meat spoilage

Procedia PDF Downloads 82

Authors: T. Topór, A. Derkowski, P. Ziemiański

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Formation of organic matter (OM)-hosted nanopores upon thermal maturation are one of the key factor controlling methane storage potential in unconventional shale-gas reservoirs. In this study, the subcritical CO₂ and N₂ gas adsorption measurements combined with scanning electron microscopy and supercritical methane adsorption have been used to characterize pore system and methane storage potential in black shales from the Baltic Basin (Poland). The samples were collected from a virtually equivalent Llandovery strata across the basin and represent a complete digenetic sequence, from thermally immature to overmature. The results demonstrate that the thermal maturation is a dominant mechanism controlling the formation of OM micro- and mesopores in the Baltic Basin shales. The formation of micro- and mesopores occurs in the oil window (vitrinite reflectance; leavedVR; ~0.5-0.9%) as a result of oil expulsion from kerogenleft OM highly porous. The generated hydrocarbons then turn into solid bitumen causing pore blocking and substantial decrease in micro- and mesopore volume in late-mature shales (VR ~0.9-1.2%). Both micro- and mesopores are regenerated in a middle of the catagenesis range (VR 1.4-1.9%) due to secondary cracking of OM and gas formation. The micropore volume in investigated shales is almost exclusively controlled by the OM content. The contribution of clay minerals to micropore volume is insignificant and masked by a strong contribution from OM. Methane adsorption capacity in the Baltic Basin shales is predominantly controlled by microporous OM with pores < 1.5 nm. The mesopore volume (2-50 nm) and mesopore surface area have no effect on methane sorption behavior. The adsorbed methane density equivalent, calculated as absolute methane adsorption divided by micropore volume, reviled a decrease of the methane loading potential in micropores with increasing maturity. The highest methane loading potential in micropores is observed for OM before metagenesis (VR < 2%), where the adsorbed methane density equivalent is greater than the density of liquid methane. This implies that, in addition to physical adsorption, absorption of methane in OM may occur before metagenesis. After OM content reduction using NaOCl solution methane adoption capacity substantially decreases, suggesting significantly greater adsorption potential for OM microstructure than for the clay minerals matrix.

Keywords: maturation, methane sorption, organic matter, porosity, shales

Procedia PDF Downloads 236

Authors: Arezoo Rahmani, Rinez Thapa, Juha-Matti Aalto, Petri Turhanen, Jouko Vepsalainen, Vesa-PekkaLehto, Joakim Riikonen

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Production of Scandium (Sc) is a complicated process because Sc is found only in low concentrations in ores and the concentration of Sc is very low compared with other metals. Therefore, utilization of typical extraction processes such as solvent extraction is problematic in scandium extraction. The Adsorption/desorption method can be used, but it is challenging to prepare materials, which have good selectivity, high adsorption capacity, and high stability. Therefore, efficient and environmentally friendly methods for Sc extraction are needed. In this study, the nanoporous composite material was developed for extracting Sc from an Sc ore. The nanoporous composite material offers several advantageous properties such as large surface area, high chemical and mechanical stability, fast diffusion of the metals in the material and possibility to construct a filter out of the material with good flow-through properties. The nanoporous silicon material was produced by first stabilizing the surfaces with a silicon carbide layer and then functionalizing the surface with bisphosphonates that act as metal chelators. The surface area and porosity of the material were characterized by N₂ adsorption and the morphology was studied by scanning electron microscopy (SEM). The bisphosphonate content of the material was studied by thermogravimetric analysis (TGA). The concentration of metal ions in the adsorption/desorption experiments was measured with inductively coupled plasma mass spectrometry (ICP-MS). The maximum capacity of the material was 25 µmol/g Sc at pH=1 and 45 µmol/g Sc at pH=3, obtained from adsorption isotherm. The selectivity of the material towards Sc in artificial solutions containing several metal ions was studied at pH one and pH 3. The result shows good selectivity of the nanoporous composite towards adsorption of Sc. Scandium was less efficiently adsorbed from solution leached from the ore of Sc because of excessive amounts of iron (Fe), aluminum (Al) and titanium (Ti) which disturbed the adsorption process. For example, the concentration of Fe was more than 4500 ppm, while the concentration of Sc was only three ppm, approximately 1500 times lower. Precipitation methods were developed to lower the concentration of the metals other than Sc. Optimal pH for precipitation was found to be pH 4. The concentration of Fe, Al and Ti were decreased by 99, 70, 99.6%, respectively, while the concentration of Sc decreased only 22%. Despite the large reduction in the concentration of other metals, more work is needed to further increase the relative concentration of Sc compared with other metals to efficiently extract it using the developed nanoporous composite material. Nevertheless, the developed material may provide an affordable, efficient and environmentally friendly method to extract Sc on a large scale.

Keywords: adsorption, nanoporous silicon, ore solution, scandium

Procedia PDF Downloads 146

Authors: D. Desai, J.Dixon, N. Jain, M. Datta

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Microbial infections of scalp consist of symptomatic appearances associated with seborrhoeic dermatitis, folliculitis, furuncles, carbuncles and ringworm. The main causative organisms in these scalp-based infections are bacteria like S. aureus, P. aeruginosa and a fungus M. Furfur. Allopathic treatment of these infections is available and efficient, but occasionally, topical applications have been found to cause side effects. India is known as the botanical garden of the world and considered as the epicentre for utilization of traditional drugs. Many treatments based on herb extracts are commonly used in India. It has been observed treatment with ethnomedicines requires a higher dosage and greater time period. Additionally, repeated applications are required to obtain the full efficacy of the treatment. An attempt has been made to imbibe the traditional knowledge with nanotechnology to generate a proficient therapeutic against scalp infections. We have imbibed metallic nanoparticles with extracts from traditional medicines and propose to formulate an antimicrobial hair massager. Four commonly used herbs for treatment against scalp disorders like Zingiber officinale (ginger), Allium sativum (garlic), Azadirachta indica (neem) leaves and Citrus limon (lemon) peel was taken. 30 gms of dried homogenized powder was obtained and processed for obtaining the aqueous and ethanolic extract by soxhlet apparatus. The extract was dried and reconstituted to obtain working solution of 1mg/ml. Phytochemical analysis for the obtained extract was done. Synthesis of nanoparticles was mediated by incubating 1mM silver nitrate with extracts of various herbs to obtain silver nanoparticles. The formation of the silver nanoparticles (AgNPs) was monitored using UV-Vis spectroscopy. The AgNPs thus obtained were centrifuged and dried. The AgNPs thus formed were characterized by X Ray Diffraction, scanning electron microscopy and transmission electron microscopy. The size of the AgNPs varied from 10-20 nm and was spherical in shape. P. aeruginosa was plated on nutrient agar and comparative antibacterial activity was tested. Comparative antimicrobial potential was calculated for the extracts and the corresponding nanoconstructs. It was found AgNPs were more efficient than their aqueous and ethanolic counterparts except in the ase of C. limon. Statistical analysis was performed to validate the results obtained.

Keywords: ethnomedicine, nanoconstructs, scalp infections, Zingiber officinale

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Authors: Manuel Salado, Mikel Rincón, Arkaitz Fidalgo, Roberto Fernandez, Senentxu Lanceros-Méndez

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Lithium-ion batteries (LIBs) are a promising technology for energy storage, but they suffer from safety concerns due to the use of flammable organic solvents in their liquid electrolytes. Solid-state electrolytes (SSEs) offer a potential solution to this problem, but they have their own limitations, such as poor ionic conductivity and high interfacial resistance. The aim of this research was to develop a new type of SSE based on metal-organic frameworks (MOFs) and ionic liquids (ILs). MOFs are porous materials with high surface area and tunable electronic properties, making them ideal for use in SSEs. ILs are liquid electrolytes that are non-flammable and have high ionic conductivity. A series of MOFs were synthesized, and their electrochemical properties were evaluated. The MOFs were then infiltrated with ILs to form a quasi-solid gel and solid xerogel SSEs. The ionic conductivity, interfacial resistance, and electrochemical performance of the SSEs were characterized. The results showed that the MOF-IL SSEs had significantly higher ionic conductivity and lower interfacial resistance than conventional SSEs. The SSEs also exhibited excellent electrochemical performance, with high discharge capacity and long cycle life. The development of MOF-IL SSEs represents a significant advance in the field of solid-state electrolytes. The high ionic conductivity and low interfacial resistance of the SSEs make them promising candidates for use in next-generation LIBs. The data for this research was collected using a variety of methods, including X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopy. The data was analyzed using a variety of statistical and computational methods, including principal component analysis, density functional theory, and molecular dynamics simulations. The main question addressed by this research was whether MOF-IL SSEs could be developed that have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. The results of this research demonstrate that MOF-IL SSEs are a promising new type of solid-state electrolyte for use in LIBs. The SSEs have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. These properties make them promising candidates for use in next-generation LIBs that are safer and have higher energy densities.

Keywords: energy storage, solid-electrolyte, ionic liquid, metal-organic-framework, electrochemistry, organic inorganic plastic crystal

Procedia PDF Downloads 83

Authors: María José Bugueño, Natalia Jaime, Cristian Castro, Diego Naranjo, Guido Trautmann, Mario Pérez-Won, Vilbett Briones-Labarca

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Proteins play a crucial role in various prepared foods, including dairy products, drinks, emulsions, and ready meals. These food proteins are naturally present in food waste and byproducts. The alkaline extraction and acid precipitation method is commonly used to extract proteins from plants and animals due to its product stability, cost-effectiveness, and ease of use. This study aimed to investigate the impact of pH-shifting storage at two different pH levels on the conformational changes affecting the physicochemical and functional properties of quinoa protein isolate (QPI) and yellow shrimp byproduct protein isolate (YSPI). The QPI and YSPI were extracted using the alkaline extraction-isoelectric precipitation method. The dispersions were adjusted to pH 4 or 12, stirred for 2 hours at 20°C to achieve a uniform dispersion, and then freeze-dried. Various analyses were conducted, including flexibility (F), free sulfhydryl content (Ho), emulsifying activity (EA), emulsifying capacity (EC), water holding capacity (WHC), oil holding capacity (OHC), intrinsic fluorescence, ultraviolet spectroscopy, differential scanning calorimetry (DSC), and Fourier transform infrared spectroscopy (FTIR) to assess the properties of the protein isolates. pH-shifting at pH 11 and 12 for QPI and YSPI, respectively, significantly improved protein properties, while property modification of the samples treated under acidic conditions was less pronounced. Additionally, the pH 11 and 12 treatments significantly improved F, Ho, EA, WHC, OHC, intrinsic fluorescence, ultraviolet spectroscopy, DSC, and FTIR. The increase in Ho was due to disulfide bond disruption, which produced more protein sub-units than other treatments for both proteins. This study provides theoretical support for comprehensively elucidating the functional properties of protein isolates, promoting the application of plant proteins and marine byproducts. The pH-shifting process effectively improves the emulsifying property and stability of QPI and YSPI, which can be considered potential plant-based or marine byproduct-based emulsifiers for use in the food industry.

Keywords: quinoa protein, yellow shrimp by-product protein, physicochemical properties, structural properties

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Authors: Agnieszka Feliczak-Guzik, Paulina Szczyglewska, Izabela Nowak

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A catalyst-assisted oxidation reaction is one of the key reactions exploited by various industries. Their conductivity yields essential compounds and intermediates, such as alcohols, epoxides, aldehydes, ketones, and organic acids. Researchers are devoting more and more attention to developing active and selective materials that find application in many catalytic reactions, such as cyclohexene epoxidation. This reaction yields 1,2-epoxycyclohexane and 1,2-diols as the main products. These compounds are widely used as intermediates in the perfume industry and synthesizing drugs and lubricants. Hence, our research aimed to use hierarchical zeolites modified with transition metal ions, e.g., Nb, V, and Ta, in the epoxidation reaction of cyclohexene using microwaveheating. Hierarchical zeolites are materials with secondary porosity, mainly in the mesoporous range, compared to microporous zeolites. In the course of the research, materials based on two commercial zeolites, with Faujasite (FAU) and Zeolite Socony Mobil-5 (ZSM-5) structures, were synthesized and characterized by various techniques, such as X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and low-temperature nitrogen adsorption/desorption isotherms. The materials obtained were then used in a cyclohexene epoxidation reaction, which was carried out as follows: catalyst (0.02 g), cyclohexene (0.1 cm3), acetonitrile (5 cm3) and dihydrogen peroxide (0.085 cm3) were placed in a suitable glass reaction vessel with a magnetic stirrer inside in a microwave reactor. Reactions were carried out at 45° C for 6 h (samples were taken every 1 h). The reaction mixtures were filtered to separate the liquid products from the solid catalyst and then transferred to 1.5 cm3 vials for chromatographic analysis. The test techniques confirmed the acquisition of additional secondary porosity while preserving the structure of the commercial zeolite (XRD and low-temperature nitrogen adsorption/desorption isotherms). The results of the activity of the hierarchical catalyst modified with niobium in the cyclohexene epoxidation reaction indicate that the conversion of cyclohexene, after 6 h of running the process, is about 70%. As the main product of the reaction, 2-cyclohexanediol was obtained (selectivity > 80%). In addition to the mentioned product, adipic acid, cyclohexanol, cyclohex-2-en-1-one, and 1,2-epoxycyclohexane were also obtained. Furthermore, in a blank test, no cyclohexene conversion was obtained after 6 h of reaction. Acknowledgments The work was carried out within the project “Advanced biocomposites for tomorrow’s economy BIOG-NET,” funded by the Foundation for Polish Science from the European Regional Development Fund (POIR.04.04.00-00-1792/18-00.

Keywords: epoxidation, oxidation reactions, hierarchical zeolites, synthesis

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Authors: Choupani Andisheh, Temucin Elif Sevval, Bediz Bekir

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Due to their various advantages compared to many other drug delivery systems such as hypodermic injections and oral medications, microneedle arrays (MNAs) are a promising drug delivery system. To achieve enhanced performance of the MN, it is crucial to develop numerical models, optimization methods, and simulations. Accordingly, in this work, the optimized design of dissolvable MNAs, as well as their manufacturing, is investigated. For this purpose, a mechanical model of a single MN, having the geometry of an obelisk, is developed using commercial finite element software. The model considers the condition in which the MN is under pressure at the tip caused by the reaction force when penetrating the skin. Then, a multi-objective optimization based on non-dominated sorting genetic algorithm II (NSGA-II) is performed to obtain geometrical properties such as needle width, tip (apex) angle, and base fillet radius. The objective of the optimization study is to reach a painless and effortless penetration into the skin along with minimizing its mechanical failures caused by the maximum stress occurring throughout the structure. Based on the obtained optimal design parameters, master (male) molds are then fabricated from PMMA using a mechanical micromachining process. This fabrication method is selected mainly due to the geometry capability, production speed, production cost, and the variety of materials that can be used. Then to remove any chip residues, the master molds are cleaned using ultrasonic cleaning. These fabricated master molds can then be used repeatedly to fabricate Polydimethylsiloxane (PDMS) production (female) molds through a micro-molding approach. Finally, Polyvinylpyrrolidone (PVP) as a dissolvable polymer is cast into the production molds under vacuum to produce the dissolvable MNAs. This fabrication methodology can also be used to fabricate MNAs that include bioactive cargo. To characterize and demonstrate the performance of the fabricated needles, (i) scanning electron microscope images are taken to show the accuracy of the fabricated geometries, and (ii) in-vitro piercing tests are performed on artificial skin. It is shown that optimized MN geometries can be precisely fabricated using the presented fabrication methodology and the fabricated MNAs effectively pierce the skin without failure.

Keywords: microneedle, microneedle array fabrication, micro-manufacturing structural optimization, finite element analysis

Procedia PDF Downloads 113

Authors: Marinela Miclau, Melinda Vajda, Nicolae Miclau, Daniel Ursu

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Characterized by a simple structure, easy and low cost fabrication, the dye-sensitized solar cell (DSSC) attracted the interest of the scientific community as an attractive alternative of conventional Si-based solar cells and thin-film solar cells. Over the past 20 years, the main efforts have attempted to enhance the efficiency of n-type DSSCs, the highest efficiency record of 14.30% was achieved using the co-sensitization of two metal-free organic dyes and Co (II/III) tris(phenanthroline)-based redox electrolyte. In the last years, the development of the efficient p-type DSSC has become a research focus owing to the fact that the concept of tandem solar cell was proposed as the solution to increase the power conversion efficiency. A promising alternative for the photocathodes of p-type DSSC, cuprous (Cu2O) and cupric (CuO) oxides have been investigated because of its nontoxic nature, low cost, high natural abundance, a good absorption coefficient for visible light and a higher dielectric constant than NiO. In case of p-type DSSC based on copper oxides with I3-/I- as redox mediator, the highest conversion efficiency of 0.42% (Cu2O) and 0.03% (CuO) has achieved. Towards the increase in the performance, we have fabricated and analyzed the performance of p-type DSSC prepared with the binder-free porous Cu2O photocathodes. Porous thin film could be an attractive alternative for DSSC because of their large surface areas which enable the efficient absorption of the dyes and light. We propose a simple and one-step hydrothermal method for the preparation of porous Cu2O thin film using copper substrate, cupric acetate and ethyl cellulose. The cubic structure of Cu2O has been determined by X-ray diffraction (XRD) and porous morphology of thin film was emphasized by Scanning Electron Microscope Inspect S (SEM). Optical and Mott-Schottky measurements attest of the high quality of the Cu2O thin film. The binder-free porous Cu2O photocathode has confirmed the excellent photovoltaic properties, the best value reported for p-type DSSC (1%) in similar conditions being reached.

Keywords: cuprous oxide, dye-sensitized solar cell, hydrothermal method, porous photocathode

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Authors: M. F. Perez, Ysmael Verde, B. Escobar, R. Barbosa, J. C. Cruz

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Reinforced concrete is one of the most important materials in the construction industry. However, in recent years the durability of concrete structures has been a worrying problem, mainly due to corrosion of reinforcing steel; the consequences of corrosion in all cases lead to shortening of the life of the structure and decrease in quality of service. Since the emergence of this problem, they have implemented different methods or techniques to reduce damage by corrosion of reinforcing steel in concrete structures; as the use of polymeric materials as coatings for the steel rod, spiked inhibitors of concrete during mixing, among others, presenting different limitations in the application of these methods. Because of this, it has been used a method that has proved effective, cathodic protection. That is why due to the properties attributed to carbon nanotubes (CNT), these could act as cathodic corrosion protection. Mounting a three-electrode electrochemical cell, carbon steel as working electrode, saturated calomel electrode (SCE) as the reference electrode, and a graphite rod as a counter electrode to close the system is performed. Samples made were subjected to a cycling process in order to compare the results in the corrosion performance of a coating composed of CNT and the others based on an anticorrosive commercial painting. The samples were tested at room temperature using an electrolyte consisting NaCl and NaOH simulating the typical pH of concrete, ranging from 12.6 to 13.9. Three test samples were made of steel rod, white, with commercial anticorrosive paint and CNT based coating; delimiting the work area to a section of 0.71 cm2. Tests cyclic voltammetry and linear voltammetry electrochemical spectroscopy each impedance of the three samples were made with a window of potential vs SCE 0.7 -1.7 a scan rate of 50 mV / s and 100 mV / s. The impedance values were obtained by applying a sine wave of amplitude 50 mV in a frequency range of 100 kHz to 100 MHz. The results obtained in this study show that the CNT based coating applied to the steel rod considerably decreased the corrosion rate compared to the commercial coating of anticorrosive paint, because the Ecorr was passed increase as the cycling process. The samples tested in all three cases were observed by light microscopy throughout the cycling process and micrographic analysis was performed using scanning electron microscopy (SEM). Results from electrochemical measurements show that the application of the coating containing carbon nanotubes on the surface of the steel rod greatly increases the corrosion resistance, compared to commercial anticorrosive coating.

Keywords: anticorrosive, carbon nanotubes, corrosion, steel

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Authors: Erin M. Durke, Monica L. McEntee, Meilu He, Suresh Dhaniyala

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Aerosols are one of the most important and significant surfaces in the atmosphere. They can influence weather, absorption, and reflection of light, and reactivity of atmospheric constituents. A notable feature of aerosol particles is the presence of a surface charge, a characteristic imparted via the aerosolization process. The existence of charge can complicate the interrogation of aerosol particles, so many researchers remove or neutralize aerosol particles before characterization. However, the charge is present in real-world samples, and likely has an effect on the physical and chemical properties of an aerosolized material. In our studies, we aerosolized different materials in an attempt to characterize the charge imparted via the aerosolization process and determine what impact it has on the aerosolized materials’ properties. The metal oxides, TiO₂ and SiO₂, were aerosolized expulsively and then characterized, using several different techniques, in an effort to determine the surface charge imparted upon the particles via the aerosolization process. Particle charge distribution measurements were conducted via the employment of a custom scanning mobility particle sizer. The results of the charge distribution measurements indicated that expulsive generation of 0.2 µm SiO₂ particles produced aerosols with upwards of 30+ charges on the surface of the particle. Determination of the degree of surface charging led to the use of non-traditional techniques to explore the impact of additional surface charge on the overall reactivity of the metal oxides, specifically TiO₂. TiO₂ was aerosolized, again expulsively, onto a gold-coated tungsten mesh, which was then evaluated with transmission infrared spectroscopy in an ultra-high vacuum environment. The TiO₂ aerosols were exposed to O₂, H₂, and CO, respectively. Exposure to O₂ resulted in a decrease in the overall baseline of the aerosol spectrum, suggesting O₂ removed some of the surface charge imparted during aerosolization. Upon exposure to H₂, there was no observable rise in the baseline of the IR spectrum, as is typically seen for TiO₂, due to the population of electrons into the shallow trapped states and subsequent promotion of the electrons into the conduction band. This result suggests that the additional charge imparted via aerosolization fills the trapped states, therefore no rise is seen upon exposure to H₂. Dosing the TiO₂ aerosols with CO showed no adsorption of CO on the surface, even at lower temperatures (~100 K), indicating the additional charge on the aerosol surface prevents the CO molecules from adsorbing to the TiO₂ surface. The results observed during exposure suggest that the additional charge imparted via aerosolization impacts the interaction with each probe gas.

Keywords: aerosols, charge, reactivity, infrared

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Authors: Faraj M. Elkhatri, Hana Ali Allafi

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The spatial and temporal distribution of diagenetic alterations related impact on the reservoir quality of the Sarir Formation. (present day burial depth of about 9000 feet) Depositional facies and diagenetic alterations are the main controls on reservoir quality of Sarir Formation Sirt Ba-sin Libya; these based on lithology and grain size as well as authigenic clay mineral types and their distributions. However, petrology investigation obtained on study area with five sandstone wells concentrated on main rock components and the parameters that may have impacts on reservoirs. the main authigenic clay minerals are kaolinite and dickite, these investigations have confirmed by X.R.D analysis and clay fraction. mainly Kaolinite and Dickite were extensively presented on all of wells with high amounts. As well as trace of detrital smectite and less amounts of illitized mud-matrix are possibly find by SEM image. Thin layers of clay presented as clay-grain coatings in local depth interpreted as remains of dissolved clay matrix is partly transformed into kaolinite adjacent and towards pore throat. This also may have impacts on most of the pore throats of this sandstone which are open and relatively clean with some of fine martial have been formed on occluded pores. This material is identified by EDS analysis to be collections of not only kaolinite booklets, but also small, disaggregated kaolinite platelets derived from the dis-aggregation of larger kaolinite booklets. These patches of kaolinite not only fill this pore, but also coat some of the sur-rounding framework grains. Quartz grains often enlarged by authigenic quartz overgrowths partially occlude and re-duce porosity. Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM) was conducted on the post-test samples to examine any mud filtrate particles that may be in the pore throats. Semi-qualitative elemental data on select-ed minerals observed during the SEM study were obtained using an Energy Dispersive Spectroscopy (EDS) unit. The samples showed mostly clean open pore throats, with limited occlusion by kaolinite.

Keywords: por throat, formation damage, porosity lose, solids plugging

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Zoltán Erdélyi, Imre Miklós Szilágyi

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Metal oxide inverse opals are a unique class of photocatalysts with a hierarchical structure that mimics the natural opal gemstone. They are composed of a network of interconnected pores, which provides a large surface area and efficient pathways for the transport of light and reactants. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. ALD allows for precise control over the thickness, composition, and morphology of the synthesized films, making it an ideal technique for the fabrication of photocatalysts with tailored properties. In this study, we report the synthesis of TiO2, ZnO, and Al2O3 inverse opal photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al2O3 can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. For example, they can be used to remove organic pollutants from wastewater, decompose harmful gases in the air, and produce hydrogen fuel from water.

Keywords: ALD, metal oxide inverse opals, composites, photocatalysis

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Authors: Franklin Chu Buh, Irene Ule Ngole Sumbele, Andrew I. R. Maas, Mathieu Motah, Jogi V. Pattisapu, Eric Youm, Basil Kum Meh, Firas H. Kobeissy, Kevin W. Wang, Peter J. A. Hutchinson, Germain Sotoing Taiwe

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Introduction: Studying TBI characteristics and their relation to outcomes can identify initiatives to improve TBI prevention and care. The objective of this study was to define the features and outcomes of TBI patients seen over a 1-year period in a level-I trauma center in Cameroon. Methods: Data on demographics, causes, injury mechanisms, clinical aspects, and discharge status were prospectively collected over a period of 12 months. The Glasgow Outcome Scale-Extended (GOSE) and the Quality of Life Questionnaire after Brain Injury (QoLIBRI) were used to evaluate outcomes 6-months after TBI. Categorical variables were described as frequencies and percentages. Comparisons between 2 categorical variables were done using Pearson's Chi-square test or Fisher's exact test. Results: A total of 160 TBI patients participated in the study. The age group 15-45 years (78%; 125) was most represented. Males were more affected (90%; 144). Low educational level was recorded in 122 (76%) cases. Road traffic incidents (RTI) were the main cause of TBI (85%), with professional bike riders being frequently involved (27%, 43/160). Assaults (7.5%) and falls (2.5%) represent the second and third most common causes of TBI in Cameroon, respectively. Only 15 patients were transported to the hospital by ambulance, and 14 of these were from a referring hospital. CT-imaging was performed in 78% (125/160) of cases intracranial traumatic abnormality was identified in 77/125 (64%) cases. Financial constraints were the main reason for not performing a CT scan on 35 patients. A total of 46 (33%) patients were discharged against medical advice (DAMA) due to financial constraints. Mortality was 14% (22/160) but disproportionately high in patients with severe TBI (46%). DAMA had poor outcomes with QoLIBRI. Only 4 patients received post-injury physiotherapy services. Conclusion: TBI in Cameroon mainly results from RTIs and commonly affects young adult males, and low educational or socioeconomic status and commercial bike riding appear to be predisposing factors. Lack of pre-hospital care, financial constraints limiting both CT-scanning and medical care, and lack of acute physiotherapy services likely influenced care and outcomes adversely.

Keywords: characteristics, traumatic brain injury, outcome, disparities in care, prospective study

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Authors: Vimal Kumar Dewangan, T. S. Sampath Kumar, Mukesh Doble, Viju Daniel Varghese

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The apatite-based, i.e., calcium-deficient hydroxyapatite (CDHAp) bone cement is well-known potential bone graft/substitute in orthopaedics due to its similar chemical composition with natural bone minerals. Therefore, an easy approach was attempted to fabricate the apatite-based (CDHAp) bone cement with improved injectability, bioresorbability, and macroporosity. In this study, the desired bone cement was developed by mixing the solid phase (consisting of wet chemically synthesized nanocrystalline hydroxyapatite and commercially available (synthetic) tricalcium phosphate) and the liquid phase (consisting of cement binding accelerator with few biopolymers in a dilute acidic solution) along with a liquid porogen as polysorbate or a solid porogen as mannitol (for comparison) in an optimized liquid-to-powder ratio. The fabricated cement sets within clinically preferred setting time (≤20 minutes) are better injectable (>70%) and also stable at ~7.3-7.4 (physiological pH). The CDHAp phased bone cement was resulted by immersing the fabricated after-set cement in phosphate buffer solution and other similar artificial body fluids and incubated at physiological conditions for seven days, confirmed through the X-ray diffraction and Fourier transform-infrared spectroscopy analyses. The so-formed synthetic apatite-based bone cement holds the acceptable compressive strength (within the range of trabecular bone) with average interconnected pores size falls in a macropores range (~50-200μm) inside the cement, verified by scanning electron microscopy (SEM), mercury intrusion porosimetry and micro-CT analysis techniques. Also, it is biodegradable (degrades ~19-22% within 10-12 weeks) when incubated in artificial body fluids under physiological conditions. The biocompatibility study of the bone cement, when incubated with MG63 cells, shows a significant increase in the cell viability after 3rd day of incubation compared with the control, and the cells were well-attached and spread completely on the surface of the bone cement, confirmed through SEM and fluorescence microscopy analyses. With this all, we can conclude that the developed synthetic macroporous apatite-based bone cement may have the potential to become promising material used as a trabecular bone substitute.

Keywords: calcium deficient hydroxyapatite, synthetic apatite-based bone cement, injectability, macroporosity, trabecular bone substitute

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Authors: Nurhafizah Md. Disa, Nurhayati Binti Abdullah, Muhammad Rabie Bin Omar

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This research intends to identify the existing knowledge gap because of the lack of substantial studies to fabricate and characterize bio-graphene created from Oil Palm Shell (OPS) through the means of pre-treatment and slow pyrolysis. By fabricating bio-graphene through OPS, a novel material can be found to procure and used for graphene-based research. The characterization of produced bio-graphene is intended to possess a unique hexagonal graphene pattern and graphene properties in comparison to other previously fabricated graphene. The OPS will be fabricated by pre-treatment of zinc chloride (ZnCl₂) and iron (III) chloride (FeCl3), which then induced the bio-graphene thermally by slow pyrolysis. The pyrolizer's final temperature and resident time will be set at 550 °C, 5/min, and 1 hour respectively. Finally, the charred product will be washed with hydrochloric acid (HCL) to remove metal residue. The obtained bio-graphene will undergo different analyses to investigate the physicochemical properties of the two-dimensional layer of carbon atoms with sp2 hybridization hexagonal lattice structure. The analysis that will be taking place is Raman Spectroscopy (RAMAN), UV-visible spectroscopy (UV-VIS), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), and X-Ray Diffraction (XRD). In retrospect, RAMAN is used to analyze three key peaks found in graphene, namely D, G, and 2D peaks, which will evaluate the quality of the bio-graphene structure and the number of layers generated. To compare and strengthen graphene layer resolves, UV-VIS may be used to establish similar results of graphene layer from last layer analysis and also characterize the types of graphene procured. A clear physical image of graphene can be obtained by analyzation of TEM in order to study structural quality and layers condition and SEM in order to study the surface quality and repeating porosity pattern. Lastly, establishing the crystallinity of the produced bio-graphene, simultaneously as an oxygen contamination factor and thus pristineness of the graphene can be done by XRD. In the conclusion of this paper, this study is able to obtain bio-graphene through OPS as a novel material in pre-treatment by chloride ZnCl₂ and FeCl3 and slow pyrolization to provide a characterization analysis related to bio-graphene that will be beneficial for future graphene-related applications. The characterization should yield similar findings to previous papers as to confirm graphene quality.

Keywords: oil palm shell, bio-graphene, pre-treatment, slow pyrolysis

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Authors: S. Z. A. Zaidi, A. Crosky

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Biocomposites is a field that has gained much scientific attention due to the current substantial consumption of non-renewable resources and the environmentally harmful disposal methods required for traditional polymer composites. Research on natural fiber reinforced polyhydroxyalkanoates (PHAs) has gained considerable momentum over the past decade. There is little work on PHAs reinforced with unidirectional (UD) natural fibers and little work on using epoxidized natural rubber (ENR) as a toughening agent for PHA-based biocomposites. In this work, we prepared polyhydroxybutyrate-co-valerate (PHBV) biocomposites reinforced with UD 30 wt.% flax fibers and evaluated the use of ENR with 50% epoxidation (ENR50) as a toughening agent for PHBV biocomposites. Quasi-unidirectional flax/PHBV composites were prepared by hand layup, powder impregnation followed by compression molding.  Toughening agents – polybutylene adiphate-co-terephthalate (PBAT) and ENR50 – were cryogenically ground into powder and mechanically mixed with main matrix PHBV to maintain the powder impregnation process. The tensile, flexural and impact properties of the biocomposites were measured and morphology of the composites examined using optical microscopy (OM) and scanning electron microscopy (SEM). The UD biocomposites showed exceptionally high mechanical properties as compared to the results obtained previously where only short fibers have been used. The improved tensile and flexural properties were attributed to the continuous nature of the fiber reinforcement and the increased proportion of fibers in the loading direction. The improved impact properties were attributed to a larger surface area for fiber-matrix debonding and for subsequent sliding and fiber pull-out mechanisms to act on, allowing more energy to be absorbed. Coating cryogenically ground ENR50 particles with PHBV powder successfully inhibits the self-healing nature of ENR-50, preventing particles from coalescing and overcoming problems in mechanical mixing, compounding and molding. Cryogenic grinding, followed by powder impregnation and subsequent compression molding is an effective route to the production of high-mechanical-property biocomposites based on renewable resources for high-obsolescence applications such as plastic casings for consumer electronics.

Keywords: natural fibers, natural rubber, polyhydroxyalkanoates, unidirectional

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Authors: Saad Mohamed Elsaid, Nabil Anwar, Mahmoud Rushdi

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One of the reasons for the intensive use of pesticides is to protect agricultural crops and orchards from pests or agricultural worms. The period of time that pesticides stay inside the soil is estimated at about (2) to (12) weeks. Perhaps the most important reason that led to groundwater pollution is the easy leakage of these harmful pesticides from the soil into the aquifers. This research aims to find the best ways to use traded activated charcoal with gold nitrate solution; for removing the deadly pesticides from the aqueous solution by adsorption phenomenon. The most used pesticides in Egypt were selected, such as Malathion, Methomyl Abamectin and, Thiamethoxam. Activated charcoal doped with gold ions was prepared by applying chemical and thermal treatments to activated charcoal using gold nitrate solution. Adsorption of studied pesticide onto activated carbon /Au was mainly by chemical adsorption, forming a complex with the gold metal immobilized on activated carbon surfaces. In addition, the gold atom was considered as a catalyst to cracking the pesticide molecule. Gold activated charcoal is a low cost material due to the use of very low concentrations of gold nitrate solution. its notice the great ability of activated charcoal in removing selected pesticides due to the presence of the positive charge of the gold ion, in addition to other active groups such as functional oxygen and lignin cellulose. The presence of pores of different sizes on the surface of activated charcoal is the driving force for the good adsorption efficiency for the removal of the pesticides under study The surface area of the prepared char as well as the active groups, were determined using infrared spectroscopy and scanning electron microscopy. Some factors affecting the ability of activated charcoal were applied in order to reach the highest adsorption capacity of activated charcoal, such as the weight of the charcoal, the concentration of the pesticide solution, the time of the experiment, and the pH. Experiments showed that the maximum limit revealed by the batch adsorption study for the adsorption of selected insecticides was in contact time (80) minutes at pH (7.70). These promising results were confirmed, and by establishing the practical application of the developed system, the effect of various operating factors with equilibrium, kinetic and thermodynamic studies is evident, using the Langmuir application on the effectiveness of the absorbent material with absorption capacities higher than most other adsorbents.

Keywords: waste water, pesticides pollution, adsorption, activated carbon

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Authors: Damian Stanislaw Nakonieczny, Grazyna Simha Martynkova, Marianna Hundakova, G. Kratosová, Karla Cech Barabaszova

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The main aim of the research was to functionalize the surface of spherical aluminum silicates in the form of so-called cenospheres. Cenospheres are light ceramic particles with a density between 0.45 and 0.85 kgm-3 hat can be obtained as a result of separation from fly ash from coal combustion. However, their occurrence is limited to about 1% by weight of dry ash mainly derived from anthracite. Hence they are very rare and desirable material. Cenospheres are characterized by complete chemical inertness. Mohs hardness in range of 6 and completely smooth surface. Main idea was to prepare the surface by chemical etching, among others hydrofluoric acid (HF) and hydrogen peroxide, caro acid, silanization using (3-aminopropyl) triethoxysilane (APTES) and tetraethyl orthosilicate (TEOS) to obtain the maximum development and functionalization of the surface to improve chemical and mechanical connection with biomedically used polymers, i.e., polyacrylic methacrylate (PMMA) and polyetheretherketone (PEEK). These polymers are used medically mainly as a material for fixed and removable dental prostheses and PEEK spinal implants. The problem with their use is the decrease in mechanical properties over time and bacterial infections fungal during implantation and use of dentures. Hence, the use of a ceramic filler that will significantly improve the mechanical properties, improve the fluidity of the polymer during shape formation, and in the future, will be able to support bacteriostatic substances such as silver and zinc ions seem promising. In order to evaluate our laboratory work, several instrumental studies were performed: chemical composition and morphology with scanning electron microscopy with Energy-Dispersive X-Ray Probe (SEM/EDX), determination of characteristic functional groups of Fourier Transform Infrared Spectroscopy (FTIR), phase composition of X-ray Diffraction (XRD) and thermal analysis of Thermo Gravimetric Analysis/differentia thermal analysis (TGA/DTA), as well as assessment of isotherm of adsorption with Brunauer-Emmett-Teller (BET) surface development. The surface was evaluated for the future application of additional bacteria and static fungus layers. Based on the experimental work, it was found that orated methods can be suitable for the functionalization of the surface of cenosphere ceramics, and in the future it can be suitable as a bacteriostatic filler for biomedical polymers, i.e., PEEK or PMMA.

Keywords: bioceramics, composites, functionalization, surface development

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Authors: Nélio Veiga, Paula Ferreira, Tiago Correia, Maria J. Correia, Carlos Pereira, Odete Amaral, Ilídio J. Correia

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Introduction: The application of fissure sealants is considered to be an important primary prevention method used in dental medicine. However, the formation of microleakage gaps between tooth enamel and the fissure sealant applied is one of the most common reasons of dental caries development in teeth with fissure sealants. The association between various dental biomaterials may limit the major disadvantages and limitations of biomaterials functioning in a complementary manner. The present study consists in the incorporation of a cariostatic agent – silver diamine fluoride (SDF) – in a resin-based fissure sealant followed by the study of release kinetics by spectrophotometry analysis of the association between both biomaterials and assessment of the inhibitory effect on the growth of the reference bacterial strain Streptococcus mutans (S. mutans) in an in vitro study. Materials and Methods: An experimental in vitro study was designed consisting in the entrapment of SDF (Cariestop^® 12% and 30%) into a commercially available fissure sealant (Fissurit^®), by photopolymerization and photocrosslinking. The same sealant, without SDF was used as a negative control. The effect of the sealants on the growth of S. mutans was determined by the presence of bacterial inhibitory halos in the cultures at the end of the incubation period. In order to confirm the absence of bacteria in the surface of the materials, Scanning Electron Microscopy (SEM) characterization was performed. Also, to analyze the release profile of SDF along time, spectrophotometry technique was applied. Results: The obtained results indicate that the association of SDF to a resin-based fissure sealant may be able to increase the inhibition of S. mutans growth. However, no SDF release was noticed during the in vitro release studies and no statistical significant difference was verified when comparing the inhibitory halo sizes obtained for test and control group.  Conclusions: In this study, the entrapment of SDF in the resin-based fissure sealant did not potentiate the antibacterial effect of the fissure sealant or avoid the immediate development of dental caries. The development of more laboratorial research and, afterwards, long-term clinical data are necessary in order to verify if this association between these biomaterials is effective and can be considered for being used in oral health management. Also, other methodologies for associating cariostatic agents and sealant should be addressed.

Keywords: biomaterial, fissure sealant, primary prevention, silver diamine fluoride

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Authors: Mohammad Khoshini, Arman Khoshghalb, Meghdad Payan, Nasser Khalili

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Most of the Earth’s crust surface rocks are technically categorized as weak rocks or weakly bonded geomaterials. Deeply weathered, weakly cemented, friable and easily erodible, they demonstrate complex material behaviour and understanding the overlooked mechanical behaviour of such materials is of particular importance in geotechnical engineering practice. Weakly bonded geomaterials are so susceptible to surface shear and moisture that conventional methods of core drilling fail to extract high-quality undisturbed samples out of them. Moreover, most of these geomaterials are of high heterogeneity rendering less reliable and feasible material characterization. In order to compensate for the unpredictability of the material response, either numerous experiments are needed to be conducted or large factors of safety must be implemented in the design process. However, none of these approaches is sustainable. In this study, a method for dry core drilling of such materials is introduced to take high-quality undisturbed core samples. By freezing the material at certain moisture content, a secondary structure is developed throughout the material which helps the whole structure to remain intact during the core drilling process. Moreover, to address the heterogeneity issue, the natural material was reconstructed artificially to obtain a homogeneous material with very high similarity to the natural one in both micro and macro-mechanical perspectives. The method is verified for both micro and macro scale. In terms of micro-scale analysis, using Scanning Electron Microscopy (SEM), pore spaces and inter-particle bonds were investigated and compared between natural and artificial materials. X-Ray Diffraction, XRD, analyses are also performed to control the chemical composition. At the macro scale, several uniaxial compressive strength tests, as well as triaxial tests, were performed to verify the similar mechanical response of the materials. A high level of agreement is observed between micro and macro results of natural and artificially bonded geomaterials. The proposed methods can play an important role to cut down the costs of experimental programs for material characterization and also to promote the accuracy of the numerical modellings based on the experimental results.

Keywords: Artificial geomaterial, core drilling, macro-mechanical behavior, micro-scale, sample preparation, SEM photography, weakly bonded geomaterials

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Authors: Sudip Mondal, Biswanath Mondal, Sudit S. Mukhopadhyay, Apurba Dey

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Bioactive materials improve devices for a long lifespan but have mechanical limitations. Mechanical characterization is one of the very important characteristics to evaluate the life span and functionality of the scaffold material. After implantation of scaffold material the primary stage rejection of scaffold occurs due to non biocompatible effect of host body system. The second major problems occur due to the effect of mechanical failure. The mechanical and biocompatibility failure of the scaffold materials can be overcome by the prior evaluation of the scaffold materials. In this study chemically treated Labeo rohita scale is used for synthesizing hydroxyapatite (HAp) biomaterial. Thermo-gravimetric and differential thermal analysis (TG-DTA) is carried out to ensure thermal stability. The chemical composition and bond structures of wet ball-milled calcined HAp powder is characterized by Fourier Transform Infrared spectroscopy (FTIR), X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Transmission Electron Microscopy (TEM), Energy Dispersive X-ray (EDX) analysis. Fish scale derived apatite materials consists of nano-sized particles with Ca/P ratio of 1.71. The biocompatibility through cytotoxicity evaluation and MTT assay are carried out in MG63 osteoblast cell lines. In the cell attachment study, the cells are tightly attached with HAp scaffolds developed in the laboratory. The result clearly suggests that HAp material synthesized in this study do not have any cytotoxic effect, as well as it has a natural binding affinity for mammalian cell lines. The synthesized HAp powder further successfully used to develop porous scaffold material with suitable mechanical property of ~0.8GPa compressive stress, ~1.10 GPa a hardness and ~ 30-35% porosity which is acceptable for implantation in trauma region for animal model. The histological analysis also supports the bio-affinity of processed HAp biomaterials in Wistar rat model for investigating the contact reaction and stability at the artificial or natural prosthesis interface for biomedical function. This study suggests the natural sourced fish scale-derived HAp material could be used as a suitable alternative biomaterial for tissue engineering application in near future.

Keywords: biomaterials, hydroxyapatite, scaffold, mechanical property, tissue engineering

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Authors: Xin Li, Zhenxue Jiang, Zhuo Li

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Generally, shale gas is trapped within shale systems with low porosity and ultralow permeability as free and adsorbing states. Its production is controlled by properties, in terms of occurrence phases, gas contents, and percolation characteristics. These properties are all influenced by porous features. In this paper, porosity differences of marine shales were explored between Lower Cambrian shale and Lower Silurian shale of Sichuan Basin, South China. Both the two shales were marine shales with abundant oil-prone kerogen and rich siliceous minerals. Whereas Lower Cambrian shale (3.56% Ro) possessed a higher thermal degree than that of Lower Silurian shale (2.31% Ro). Samples were measured by a combination of organic-chemistry geology measurement, organic matter (OM) isolation, X-ray diffraction (XRD), N2 adsorption, and focused ion beam milling and scanning electron microscopy (FIB-SEM). Lower Cambrian shale presented relatively low pore properties, with averaging 0.008ml/g pore volume (PV), averaging 7.99m²/g pore surface area (PSA) and averaging 5.94nm average pore diameter (APD). Lower Silurian shale showed as relatively high pore properties, with averaging 0.015ml/g PV, averaging 10.53m²/g PSA and averaging 18.60nm APD. Additionally, fractal analysis indicated that the two shales presented discrepant pore morphologies, mainly caused by differences in the combination of pore types between the two shales. More specifically, OM-hosted pores with pin-hole shape and dissolved pores with dead-end openings were the main types in Lower Cambrian shale, while OM-hosted pore with a cellular structure was the main type in Lower Silurian shale. Moreover, porous characteristics of isolated OM suggested that OM of Lower Silurian shale was more capable than that of Lower Cambrian shale in the aspect of pore contribution. PV of isolated OM in Lower Silurian shale was almost 6.6 times higher than that in Lower Cambrian shale, and PSA of isolated OM in Lower Silurian shale was almost 4.3 times higher than that in Lower Cambrian shale. However, no apparent differences existed among samples with various matrix compositions. At late diagenetic or metamorphic epoch, extensive diagenesis overprints the effects of minerals on pore properties and OM plays the dominant role in pore developments. Hence, differences of porous features between the two marine shales highlight the effect of diagenetic degree on OM-hosted pore development. Consequently, distinctive pore characteristics may be caused by the different degrees of diagenetic evolution, even with similar matrix basics.

Keywords: marine shale, lower Cambrian, lower Silurian, om isolation, pore properties, om-hosted pore

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Authors: Mantas Sriubas, Kristina Bockute, Darius Virbukas, Giedrius Laukaitis

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In this work, the doped TiO2 (dopants – Ca, Mg) was investigated. The comparison between the physical vapour deposition methods as electron beam vapour deposition and magnetron sputtering was performed and the structural and electrical properties of the formed thin films were investigated. Thin films were deposited on different type of substrates: SiO2, Alloy 600 (Fe-Ni-Cr) and Al2O3 substrates. The structural properties were investigated using Ambios XP-200 profilometer, scanning electron microscope (SEM) Hitachi S-3400N, X-ray energy-dispersive spectroscope (EDS) Quad 5040 (Bruker AXS Microanalysis GmbH), X-ray diffractometer (XRD) D8 Discover (Bruker AXS GmbH) with glancing angles focusing geometry in a 20 – 70° range using the Cu Kα1 λ = 0.1540562 nm radiation). The impedance spectroscopy measurements were performed using Probostat® (NorECs AS) measurement cell in the frequency range from 10-1-106 Hz under reducing and oxidizing conditions in temperature range of 200 °C to 1200 °C. The investigation of the e-beam deposited Ca and Mg doped-TiO2 thin films shows that the thin films are dense without any visible pores and cavities and the thin films grow in zone T according Barna-Adamik SZM. Substrate temperature was kept 600 °C during the deposition and Ts/Tm ≈ 0.32 (substrate temperature (Ts) and coating material melting temperature (Tm)). The surface diffusion is high however, the grain boundary migration is strongly limited at this temperature. This means that structure is inhomogeneous and the columnar structure is mostly visible in the upper part of the films. According to XRD, the increasing of the Ca dopants’ concentration increases the crystallinity of the formed thin films and the crystallites size increase linearly and Ca dopants act as prohibitors. Thin films are comprised of anatase TiO2 phase with an exception of 2 % Ca doped TiO2, where a small peak of Ca arise. In the case of Mg doped-TiO2 the intensities of the XRD peaks decreases with increasing Mg molar concentration. It means that there are less diffraction planes of the particular orientation in thin films with higher impurities concentration. Thus, the crystallinity decreases with increasing Mg concentration and Mg dopants act as inhibitors. The impedance measurements show that the dopants changed the conductivity of the formed thin films. The conductivity varies from 10-3 S/cm to 10-4 S/cm at 800 °C under wet reducing conditions. The microstructure of the magnetron sputtered thin TiO2 films is different comparing to the thin films deposited using e-beam deposition therefore influencing other structural and electrical properties.

Keywords: electrical properties, electron beam deposition, magnetron sputtering, microstructure, titanium dioxide

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Authors: Raghuram Kandimalla, Sanjeeb Kalita, Bhaswati Choudhury, Jibon Kotoky

Abstract:

The quest for developing an ideal suture material prompted our interest to develop a novel suture with advantageous characteristics to market available ones. We developed novel suture biomaterial from muga silk (Antheraea assama) and ramie (Boehmeria nivea) plant fiber. Field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), attenuated total reflection fourier transform infrared spectroscopy (ATR-FTIR) and thermo gravimetric analysis (TGA) results revealed the physicochemical properties of the fibers which supports the suitability of fibers for suture fabrication. Tensile properties of the prepared sutures were comparable with market available sutures and it found to be biocompatible towards human erythrocytes and nontoxic to mammalian cells. The prepared sutures completely healed the superficial deep wound incisions within seven days in adult male wister rats leaving no rash and scar. Histopathology studies supports the wound healing ability of sutures, as rapid synthesis of collagen, connective tissue and other skin adnexal structures were observed within seven days of surgery. Further muga suture surface modified by exposing the suture to oxygen plasma which resulted in formation of nanotopography on suture surface. Broad spectrum antibiotic amoxicillin was functionalized on the suture surface to prepare an advanced antimicrobial muga suture. Surface hydrophilicity induced by oxygen plasma results in an increase in drug-impregnation efficiency of modified muga suture by 16.7%. In vitro drug release profiles showed continuous and prolonged release of amoxicillin from suture up to 336 hours. The advanced muga suture proves to be effective against growth inhibition of Staphylococcus aureus and Escherichia coli, whereas normal muga suture offers no antibacterial activity against both types of bacteria. In vivo histopathology studies and colony-forming unit count data revealed accelerated wound healing activity of advanced suture over normal one through rapid synthesis and proliferation of collagen, hair follicle and connective tissues.

Keywords: sutures, biomaterials, silk, Ramie

Procedia PDF Downloads 317

Authors: Magdalena Diaka, Paweł Mazierski, Joanna Żebrowska, Michał Winiarski, Tomasz Klimczuk, Adriana Zaleska-Medynska

Abstract:

During the last years, TiO2 nanotubes have been widely studied due to their unique highly ordered array structure, unidirectional charge transfer and higher specific surface area compared to conventional TiO2 powder. These photoactive materials, in the form of thin layer, can be activated by low powered and low cost irradiation sources (such as LEDs) to remove VOCs, microorganism and to deodorize air streams. This is possible due to their directly growth on a support material and high surface area, which guarantee enhanced photon absorption together with an extensive adsorption of reactant molecules on the photocatalyst surface. TiO2 nanotubes exhibit also lots of other attractive properties, such as potential enhancement of electron percolation pathways, light conversion, and ion diffusion at the semiconductor-electrolyte interface. Pure TiO2 nanotubes were previously used to remove organic compounds from the gas phase as well as in water splitting reaction. The major factors limiting the use of TiO2 nanotubes, which have not been fully overcome, are their relatively large band gap (3-3,2 eV) and high recombination rate of photogenerated electron–hole pairs. Many different strategies were proposed to solve this problem, however titania nanostructures containing incorporated metal oxides like Ag2O shows very promising, new optical and photocatalytic properties. Unfortunately, there is still very limited number of reports regarding application of TiO2/MxOy nanostructures. In the present work, we prepared TiO2/Ag2O nanotubes obtained by anodization of Ti-Ag alloys containing 5, 10 and 15 wt. % Ag. Photocatalysts prepared in this way were characterized by X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), luminescence spectroscopy and UV-Vis spectroscopy. The activities of new TiO2/Ag2O were examined by photocatalytic degradation of toluene in gas phase reaction and phenol in aqueous phase using 1000 W Xenon lamp (Oriel) and light emitting diodes (LED) as a irradiation sources. Additionally efficiency of bacteria (Pseudomonas aeruginosa) removal from the gas phase was estimated. The number of surviving bacteria was determined by the serial twofold dilution microtiter plate method, in Tryptic Soy Broth medium (TSB, GibcoBRL).

Keywords: photocatalysis, antibacterial properties, titania nanotubes, new TiO2/MxOy nanostructures

Procedia PDF Downloads 293