Search results for: powder x-ray diffraction

Authors: M. Sivakumar, D. Chamundeeswari

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Glycosmis pentaphylla is one of the medicinally important plants belonging to the family Rutaceae, commonly known as “Anam or Panal” in Tamil. Traditionally, leaves are useful in fever, hepatopathy, eczema, skin disease, helminthiasis, wounds, and erysipelas. The fruits are sweet and are useful in vitiated conditions of vata, kapha, cough, and bronchitis. The roots are good for facial inflammations, rheumatism, jaundice, and anemia. The preliminary phytochemical investigations indicated the presence of alkaloids, terpenoids, flavonoids, tannins, sugar, glycoside, and phenolic compounds. In the present study, the root part of Glycosmis pentaphylla was used, and the root was collected from Western Ghats of South India. The root was sun/shade dried and pulverized to powder in a mechanical grinder. The powder was successively extracted with various solvents, and the ethyl acetate extract of Glycosmis pentaphylla has been subjected to the GC-MS analysis. Amongst the 46 chemical constituents identified from this plant, three major phytoconstituents were reported for the first time. Marmesin, a furanocumarin compound with the chemical structure 7H-Furo (3,2-G) (1)Benzopyran-7-one,2,3–dihydro–2 - (1-Hydroxy-1methylethyl)-(s) is one of the three compounds identified for the first time at the concentration of 11-60% in ethyl acetate extract of Glycosmis pentaphylla. Others include, Beta.-Fagarine (4.71%) and Paverine (13.08%).

Keywords: Ethyl acetate extract, Glycosmis pentaphylla, GC-MS analysis, phytochemicals.

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Authors: Maribel G. Guzmán, Jean Dille, Stephan Godet

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Silver nanoparticles were prepared by chemical reduction method. Silver nitrate was taken as the metal precursor and hydrazine hydrate as a reducing agent. The formation of the silver nanoparticles was monitored using UV-Vis absorption spectroscopy. The UV-Vis spectroscopy revealed the formation of silver nanopart├¡cles by exhibing the typical surface plasmon absorption maxima at 418-420 nm from the UV–Vis spectrum. Comparison of theoretical (Mie light scattering theory) and experimental results showed that diameter of silver nanoparticles in colloidal solution is about 60 nm. We have used energy-dispersive spectroscopy (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and, UV–Vis spectroscopy to characterize the nanoparticles obtained. The energy-dispersive spectroscopy (EDX) of the nanoparticles dispersion confirmed the presence of elemental silver signal no peaks of other impurity were detected. The average size and morphology of silver nanoparticles were determined by transmission electron microscopy (TEM). TEM photographs indicate that the nanopowders consist of well dispersed agglomerates of grains with a narrow size distribution (40 and 60 nm), whereas the radius of the individual particles are between 10 and 20 nm. The synthesized nanoparticles have been structurally characterized by X-ray diffraction and transmission high-energy electron diffraction (HEED). The peaks in the XRD pattern are in good agreement with the standard values of the face-centered-cubic form of metallic silver (ICCD-JCPDS card no. 4-0787) and no peaks of other impurity crystalline phases were detected. Additionally, the antibacterial activity of the nanopart├¡culas dispersion was measured by Kirby-Bauer method. The nanoparticles of silver showed high antimicrobial and bactericidal activity against gram positive bacteria such as Escherichia Coli, Pseudimonas aureginosa and staphylococcus aureus which is a highly methicillin resistant strain.

Keywords: Silver nanoparticles, surface plasmon, UV-Vis absorption spectrum, chemicals reduction.

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Authors: Shams Ul Khaliq, Khan Shahzada, Bashir Alam, Fawad Bilal, Mushtaq Zeb, Faizan Akbar

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Marble industry contributes its fair share in environmental deterioration, producing voluminous amounts of mud and other excess residues obtained from marble and granite processing, polluting soil, water and air. Reusing these products in other products will not just prevent our environment from polluting but also help with economy. In this research, an attempt has been made to study the expediency of waste Marble Powder (MP) in concrete production. Various laboratory tests were performed to investigate permeability, physical and mechanical properties, such as slump, compressive strength, split tensile test, etc. Concrete test samples were fabricated with varying MP content (replacing 5-30% cement), furnished from two different sources. 5% replacement of marble dust caused 6% and 12% decrease in compressive and tensile strength respectively. These parameters gradually decreased with increasing MP content up to 30%. Most optimum results were obtained with 10% replacement. Improvement in consistency and permeability were noticed. The permeability was improved with increasing MP proportion up to 10% without substantial decrease in compressive strength. Obtained results revealed that MP as an alternative to cement in concrete production is a viable option considering its economic and environment friendly implications.

Keywords: Waste marble dust, concrete strength, environment, concrete, permeability.

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Authors: W. Thepsuwan, N. Monmaturapoj

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Calcium phosphate cement (CPC) is one of the most attractive bioceramics due to its moldable and shape ability to fill complicated bony cavities or small dental defect positions. In this study, CPC was produced by using mixture of tetracalcium phosphate (TTCP, Ca4O(PO4)2) and dicalcium phosphate anhydrous (DCPA, CaHPO4) in equimolar ratio (1/1) with aqueous solutions of acetic acid (C2H4O2) and disodium hydrogen phosphate dehydrate (Na2HPO4.2H2O) in combination with sodium alginate in order to improve theirs moldable characteristic. The concentration of the aqueous solutions and sodium alginate were varied to investigate the effect of different aqueous solutions and alginate on properties of the cements. The cement paste was prepared by mixing cement powder (P) with aqueous solution (L) in a P/L ratio of 1.0g/0.35ml. X-ray diffraction (XRD) was used to analyses phase formation of the cements. Setting time and compressive strength of the set CPCs were measured using the Gilmore apparatus and Universal testing machine, respectively. The results showed that CPCs could be produced by using both basic (Na2HPO4.2H2O) and acidic (C2H4O2) solutions. XRD results show the precipitation of hydroxyapatite in all cement samples. No change in phase formation among cements using difference concentrations of Na2HPO4.2H2O solutions. With increasing concentration of acidic solutions, samples obtained less hydroxyapatite with a high dicalcium phosphate dehydrate leaded to a shorter setting time. Samples with sodium alginate exhibited higher crystallization of hydroxyapatite than that of without alginate as a result of shorten setting time in a basic solution but a longer setting time in an acidic solution. The stronger cement was attained from samples using the acidic solution with sodium alginate; however the strength was lower than that of using the basic solution.

Keywords: Calcium phosphate cements, TTCP, DCPA, hydroxyapatite, properties.

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Authors: Amine Rezzoug, Said Abdi, Nadjet Bouhelal, Ismail Daoud

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This paper investigates the application of metallic coatings on high fiber volume fraction carbon/epoxy polymer matrix composites. For the grip of the metallic layer, a method of modifying the surface of the composite by introducing a mixture of copper and steel powder (filler powders) which can reduce the impact of thermal spray particles. The powder was introduced to the surface at the time of the forming. Arc spray was used to project the zinc coating layer. The substrate was grit blasted to avoid poor adherence. The porosity, microstructure, and morphology of layers are characterized by optical microscopy, SEM and image analysis. The samples were studied also in terms of hardness and erosion resistance. This investigation did not reveal any visible evidence damage to the substrates. The hardness of zinc layer was about 25.94 MPa and the porosity was around (∼6.70%). The erosion test showed that the zinc coating improves the resistance to erosion. Based on the results obtained, we can conclude that thermal spraying allows the production of protective coating on PMC. Zinc coating has been identified as a compatible material with the substrate. The filler powders layer protects the substrate from the impact of hot particles and allows avoiding the rupture of brittle carbon fibers.

Keywords: Arc spray, coating, composite, erosion.

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Authors: S. Srikiran, Dharmala Venkata Padmaja, P. N. L. Pavani, R. Pola Rao, K. Ramji

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Technological advancements in the development of cutting tools and coolant/lubricant chemistry have enhanced the machining capabilities of hard materials under higher machining conditions. Generation of high temperatures at the cutting zone during machining is one of the most important and pertinent problems which adversely affect the tool life and surface finish of the machined components. Generally, cutting fluids and solid lubricants are used to overcome the problem of heat generation, which is not effectively addressing the problems. With technological advancements in the field of tribology, nano-level particulate solid lubricants are being used nowadays in machining operations, especially in the areas of turning and grinding. The present investigation analyses the effect of using nano-particulate graphite powder as lubricant in the turning of AISI 1040 steel under variable machining conditions and to study its effect on cutting forces, tool temperature and surface roughness of the machined component. Experiments revealed that the increase in cutting forces and tool temperature resulting in the decrease of surface quality with the decrease in the size of nano-particulate graphite powder as lubricant.

Keywords: Solid lubricant, graphite, minimum quantity lubrication, nanoparticles.

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Authors: Rania Mustafa

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This audit was conducted at Manchester University NHS Foundation Trust, Wythenshawe Hospital Radiology and Accident and Emergency [A&E] Department to assess the appropriateness of clinical information in X-ray requests, specifically in cases of acute ankle injuries. As per the Ottawa Ankle Rules and the recommendations of National Institute for Health and Care Excellence [NICE] and the Royal College of Radiology, we aimed to evaluate the appropriateness of referrals and the thoroughness of clinical information provided by Emergency Department [ED] clinicians for ankle radiography. Our goal was to achieve 100% compliance with these guidelines. The audit involved a comprehensive analysis spanning the period from August 2022 to January 2023, encompassing patient records, radiographic orders, and clinical assessments. Data collection included patient demographics, presenting complaints, clinical assessments, adherence to Ottawa Ankle Rules criteria, and subsequent radiography orders. Here we conducted two audit cycles, involving 38 patients in the first cycle and 86 patients in the second cycle. The data were furtherly filtered to include all patients who were referred from the ED for an ankle Xray with a history of acute trauma and age of more than 18 years. The key finding was that in August 2022, 60% of cases met the Ottawa Ankle Rules criteria accurately, indicating a need for improvement in adherence. However, by January 2023, there was a notable improvement, with 95% of cases accurately meeting the criteria. This significant change reflects an increased alignment with best practices for ankle radiography referrals.

Keywords: Ankle, injuries, Ottawa Ankle Rule, X-rays.

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Authors: Reihaneh Ahmadzadeh Ghavidel, Mehdi Ghiafeh Davoodi

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The usefulness of weaning foods to meet the nutrient needs of children is well recognized, and most of them are precooked roller dried mixtures of cereal and/or legume flours which posses a high viscosity and bulk when reconstituted. The objective of this study was to formulate composite weaning foods using cereals, malted legumes and vegetable powders and analyze them for nutrients, functional properties and sensory attributes. Selected legumes (green gram and lentil) were germinated, dried and dehulled. Roasted wheat, rice, carrot powder and skim milk powder also were used. All the ingredients were mixed in different proportions to get four formulations, made into 30% slurry and dried in roller drier. The products were analyzed for proximate principles, mineral content, functional and sensory qualities. The results of analysis showed following range of constituents per 100g of formulations on dry weight basis, protein, 18.1-18.9 g ; fat, 0.78-1.36 g ; iron, 5.09-6.53 mg; calcium, 265-310 mg. The lowest water absorption capacity was in case of wheat green gram based and the highest was in rice lentil based sample. Overall sensory qualities of all foods were graded as “good" and “very good" with no significant differences. The results confirm that formulated weaning foods were nutritionally superior, functionally appropriate and organoleptically acceptable.

Keywords: malted legumes, weaning foods, nutrition, functional properties

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Authors: Sharareh Mohseni, Reihaneh Ahmadzadeh Ghavidel

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Tomato powder has good potential as substitute of tomato paste and other tomato products. In order to protect physicochemical properties and nutritional quality of tomato during dehydration process, investigation was carried out using different drying methods and pretreatments. Solar drier and continuous conveyor (tunnel) drier were used for dehydration where as calcium chloride (CaCl2), potassium metabisulphite (KMS), calcium chloride and potassium metabisulphite (CaCl2 +KMS), and sodium chloride (NaCl) selected for treatment.. lycopene content, dehydration ratio, rehydration ratio and non-enzymatic browning in addition to moisture, sugar and titrable acidity were studied. Results show that pre-treatment with CaCl2 and NaCl increased water removal and moisture mobility in tomato slices during drying of tomatoes. Where CaCl2 used along with KMS the NEB was recorded the least compared to other treatments and the best results were obtained while using the two chemicals in combination form. Storage studies in LDPE polymeric and metalized polyesters films showed less changes in the products packed in metallized polyester pouches and even after 6 months lycopene content did not decrease more than 20% as compared to the control sample and provide extension of shelf life in acceptable condition for 6 months. In most of the quality characteristics tunnel drier samples presented better values in comparison to solar drier.

Keywords: Dehydration, Tomato powder, Lycopene, Browning

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Authors: R. Ibrahim, M. Azmirruddin, M. Jabir, N. Johari, M. Muhamad, A. R. A. Talib

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Inconel718 has been widely used as a super alloy in aerospace application due to the high strength at elevated temperatures, satisfactory oxidation resistance and heat corrosion resistance. In this study, the Inconel718 has been fabricated using high technology of Metal Injection Molding (MIM) process due to the cost effective technique for producing small, complex and precision parts in high volume compared with conventional method through machining. Through MIM, the binder system is one of the most important criteria in order to successfully fabricate the Inconel718. Even though, the binder system is a temporary, but failure in the selection and removal of the binder system will affect on the final properties of the sintered parts. Therefore, the binder system based on palm oil derivative which is palm stearin has been formulated and developed to replace the conventional binder system. The rheological studies of the mixture between the powder and binders system have been determined properly in order to be successful during injection into injection molding machine. After molding, the binder holds the particles in place. The binder system has to be removed completely through debinding step. During debinding step, solvent debinding and thermal pyrolysis has been used to remove completely of the binder system. The debound part is then sintered to give the required physical and mechanical properties. The results show that the properties of the final sintered parts fulfill the Standard Metal Powder Industries Federation (MPIF) 35 for MIM parts.

Keywords: Binder system, rheological study, metal injection molding, debinding and sintered parts.

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Authors: S. Ghanaraja, Subrata Ray, S. K. Nath

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Particle reinforced Metal Matrix Composite (MMC) succeeds in synergizing the metallic matrix with ceramic particle reinforcements to result in improved strength, particularly at elevated temperatures, but adversely it affects the ductility of the matrix because of agglomeration and porosity. The present study investigates the outcome of tensile properties in a cast and hot forged composite reinforced simultaneously with coarse and fine particles. Nano-sized alumina particles have been generated by milling mixture of aluminum and manganese dioxide powders. Milled particles after drying are added to molten metal and the resulting slurry is cast. The microstructure of the composites shows good distribution of both the size categories of particles without significant clustering. The presence of nanoparticles along with coarser particles in a composite improves both strength and ductility considerably. Delay in debonding of coarser particles to higher stress is due to reduced mismatch in extension caused by increased strain hardening in presence of the nanoparticles. However, higher addition of powder mix beyond a limit results in deterioration of mechanical properties, possibly due to clustering of nanoparticles. The porosity in cast composite generally increases with the increasing addition of powder mix as observed during process and on forging it has got reduced. The base alloy and nanocomposites show improvement in flow stress which could be attributed to lowering of porosity and grain refinement as a consequence of forging.

Keywords: Aluminum, alumina, nanoparticle reinforced composites, porosity.

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Authors: Débora N. Zambrano, Marina O. Gosatti, Leandro M. Dufou, Daniel A. Serrano, M. Mónica Guraya, Soledad Perez-Catán

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Nanoporous g-Al₂O₃ samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al₂O₃. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al₂O₃ samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al₂O₃, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al₂O₃ for all samples. Also BET specific area values (253-280 m²/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.

Keywords: Nanostructure alumina, boehmite, sol-gel technique, N2 adsorption/desorption isotherm, pore size distribution, BET area.

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Authors: B. Cilek Tatar, G. Sumnu, M. Oztop, E. Ayaz

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Encapsulation protects sensitive food ingredients against heat, oxygen, moisture and pH until they are released to the system. It can mask the unwanted taste of nutrients that are added to the foods for fortification purposes. Cherry laurels (Prunus laurocerasus) contain phenolic compounds which decrease the proneness to several chronic diseases such as types of cancer and cardiovascular diseases. The objective of this research was to study the effects of centrifugation, different coating materials and homogenization methods on microencapsulation of powders obtained from cherry laurels. In this study, maltodextrin and mixture of maltodextrin:whey protein with a ratio of 1:3 (w/w) were chosen as coating materials. Total solid content of coating materials was kept constant as 10% (w/w). Capsules were obtained from powders of freeze-dried cherry laurels through encapsulation process by silent crusher homogenizer or microfluidization. Freeze-dried cherry laurels were core materials and core to coating ratio was chosen as 1:10 by weight. To homogenize the mixture, high speed homogenizer was used at 4000 rpm for 5 min. Then, silent crusher or microfluidizer was used to complete encapsulation process. The mixtures were treated either by silent crusher for 1 min at 75000 rpm or microfluidizer at 50 MPa for 3 passes. Freeze drying for 48 hours was applied to emulsions to obtain capsules in powder form. After these steps, dry capsules were grounded manually into a fine powder. The microcapsules were analyzed for total antioxidant activity with DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging method. Prior to high speed homogenization, the samples were centrifuged (4000 rpm, 1 min). Centrifugation was found to have positive effect on total antioxidant activity of capsules. Microcapsules treated by microfluidizer were found to have higher total antioxidant activities than those treated by silent crusher. It was found that increasing whey protein concentration in coating material (using maltodextrin:whey protein 1:3 mixture) had positive effect on total antioxidant activity for both silent crusher and microfluidization methods. Therefore, capsules prepared by microfluidization of centrifuged mixtures can be selected as the best conditions for encapsulation of cherry laurel powder by considering their total antioxidant activity. In this study, it was shown that capsules prepared by these methods can be recommended to be incorporated into foods in order to enhance their functionality by increasing antioxidant activity.

Keywords: Antioxidant activity, cherry laurel, microencapsulation, microfluidization.

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Authors: S. S. Sravanthi, Swati Ghosh Acharyya

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Automotive light weighting is of major prominence in the current times due to its contribution in improved fuel economy and reduced environmental pollution. Various arc welding technologies are being employed in the production of automobile components with reduced weight. The present study is of practical importance since it involves preferential substitution of Zinc coated mild steel with a light weight alloy such as 6061 Aluminium by means of Gas Metal Arc Welding (GMAW) – Brazing technique at different processing parameters. However, the fabricated joints have shown the generation of Al – Fe layer at the interfacial regions which was confirmed by the Scanning Electron Microscope and Energy Dispersion Spectroscopy. These Al-Fe compounds not only affect the mechanical strength, but also predominantly deteriorate the corrosion resistance of the joints. Hence, it is essential to understand the phases formed in this layer and their crystal structure. Micro area X - ray diffraction technique has been exclusively used for this study. Moreover, the crevice corrosion analysis at the joint interfaces was done by exposing the joints to 5 wt.% FeCl₃ solution at regular time intervals as per ASTM G 48-03. The joints have shown a decreased crevice corrosion resistance with increased heat intensity. Inner surfaces of welds have shown severe oxide cracking and a remarkable weight loss when exposed to concentrated FeCl₃. The weight loss was enhanced with decreased filler wire feed rate and increased heat intensity. 

Keywords: Automobiles, welding, corrosion, lap joints, Micro XRD.

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Authors: S. A. Razavi Alavi, M. Torabi Angaji, Z. Gholami

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In the process of polyethylene extrusion polymer material similar to powder or granule is under compression, melting and transmission operation and on base of special form, extrudate has been produced. Twin-screw extruders are applicable in industries because of their high capacity. The powder mixing with chemical additives and melting with thermal and mechanical energy in three zones (feed, compression and metering zone) and because of gear pump and screw's pressure, converting to final product in latest plate. Extruders with twin-screw and short distance between screws are better than other types because of their high capacity and good thermal and mechanical stress. In this paper, process of polyethylene extrusion and various tapes of extruders are studied. It is necessary to have an exact control on process to producing high quality products with safe operation and optimum energy consumption. The granule size is depending on granulator motor speed. Results show at constant feed rate a decrease in granule size was found whit Increase in motor speed. Relationships between HDPE feed rate and speed of granulator motor, main motor and gear pump are calculated following as: x = HDPE feed flow rate, yM = Main motor speed yM = (-3.6076e-3) x^4+ (0.24597) x^3+ (-5.49003) x^2+ (64.22092) x+61.66786 (1) x = HDPE feed flow rate, yG = Gear pump speed yG = (-2.4996e-3) x^4+ (0.18018) x^3+ (-4.22794) x^2+ (48.45536) x+18.78880 (2) x = HDPE feed flow rate, y = Granulator motor speed 10th Degree Polynomial Fit: y = a+bx+cx^2+dx^3... (3) a = 1.2751, b = 282.4655, c = -165.2098, d = 48.3106, e = -8.18715, f = 0.84997 g = -0.056094, h = 0.002358, i = -6.11816e-5 j = 8.919726e-7, k = -5.59050e-9

Keywords: Extrusion, Extruder, Granule, HDPE, Polymer, Twin-Screw extruder.

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Authors: D. Berdous, H. Ferfera-Harrar

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Superabsorbent polymers (SAPs) or hydrogels with three-dimensional hydrophilic network structure are high-performance water absorbent and retention materials. The in situ synthesis of metal nanoparticles within polymeric network as antibacterial agents for bio-applications is an approach that takes advantage of the existing free-space into networks, which not only acts as a template for nucleation of nanoparticles, but also provides long term stability and reduces their toxicity by delaying their oxidation and release. In this work, SAP/nanosilver nanocomposites were successfully developed by a unique green process at room temperature, which involves in situ formation of silver nanoparticles (AgNPs) within hydrogels as a template. The aim of this study is to investigate whether these AgNPs-loaded hydrogels are potential candidates for antimicrobial applications. Firstly, the superabsorbents were prepared through radical copolymerization via grafting and crosslinking of acrylamide (AAm) onto chitosan backbone (Cs) using potassium persulfate as initiator and N,N’-methylenebisacrylamide as the crosslinker. Then, they were hydrolyzed to achieve superabsorbents with ampholytic properties and uppermost swelling capacity. Lastly, the AgNPs were biosynthesized and entrapped into hydrogels through a simple, eco-friendly and cost-effective method using aqueous silver nitrate as a silver precursor and curcuma longa tuber-powder extracts as both reducing and stabilizing agent. The formed superabsorbents nanocomposites (Cs-g-PAAm)/AgNPs were characterized by X-ray Diffraction (XRD), UV-visible Spectroscopy, Attenuated Total reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR), Inductively Coupled Plasma (ICP), and Thermogravimetric Analysis (TGA). Microscopic surface structure analyzed by Transmission Electron Microscopy (TEM) has showed spherical shapes of AgNPs with size in the range of 3-15 nm. The extent of nanosilver loading was decreased by increasing Cs content into network. The silver-loaded hydrogel was thermally more stable than the unloaded dry hydrogel counterpart. The swelling equilibrium degree (Q) and centrifuge retention capacity (CRC) in deionized water were affected by both contents of Cs and the entrapped AgNPs. The nanosilver-embedded hydrogels exhibited antibacterial activity against Escherichia coli and Staphylococcus aureus bacteria. These comprehensive results suggest that the elaborated AgNPs-loaded nanomaterials could be used to produce valuable wound dressing.

Keywords: Antibacterial activity, nanocomposites, silver nanoparticles, superabsorbent hydrogel.

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Authors: M. Ferguson, T. Konkova, I. Violatos

Abstract:

Microstructure analysis of additively manufactured (AM) materials is an important step in understanding the interrelationship between mechanical properties and materials performance. Literature on the effect of a laser-based AM process parameters on the microstructure in the substrate-deposit interface is limited. The interface region, the adjoining area of substrate and deposit, is characterized by the presence of the fusion zone (FZ) and heat affected zone (HAZ) experiencing rapid thermal gyrations resulting in thermal induced transformations. Inconel 718 was utilized as a work material for both the substrate and deposit. Three blocks of Inconel 718 material were deposited by Direct Energy Deposition (DED) using three different laser powers, 550W, 750W and 950W, respectively. A coupled thermo-mechanical transient approach was utilized to correlate temperature history to the evolution of microstructure. Thermal history of the deposition process was monitored with the thermocouples installed inside the substrate material. Interface region of the blocks were analysed with Optical Microscopy (OM) and Scanning Electron Microscopy (SEM) including electron back-scattered diffraction (EBSD) technique. Laser power was found to influence the dissolution of intermetallic precipitated phases in the substrate and grain growth in the interface region. Microstructure and thermal history data were utilized to draw conclusive comparisons between the investigated process parameters.

Keywords: Additive manufacturing, direct energy deposition, electron back-scatter diffraction, finite element analysis, Inconel 718, microstructure, optical microscopy, scanning electron microscopy, substrate-deposit interface region.

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Authors: M. M. Hasan, A. S. M. A. Haseeb, R. Saidur, H. H. Masjuki

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In this investigation, anatase TiO2 thin films were grown by radio frequency magnetron sputtering on glass substrates at a high sputtering pressure and room temperature. The anatase films were then annealed at 300-600 °C in air for a period of 1 hour. To examine the structure and morphology of the films, X-ray diffraction (XRD) and atomic force microscopy (AFM) methods were used respectively. From X-ray diffraction patterns of the TiO2 films, it was found that the as-deposited film showed some differences compared with the annealed films and the intensities of the peaks of the crystalline phase increased with the increase of annealing temperature. From AFM images, the distinct variations in the morphology of the thin films were also observed. The optical constants were characterized using the transmission spectra of the films obtained by UV-VIS-IR spectrophotometer. Besides, optical thickness of the film deposited at room temperature was calculated and cross-checked by taking a cross-sectional image through SEM. The optical band gaps were evaluated through Tauc model. It was observed that TiO2 films produced at room temperatures exhibited high visible transmittance and transmittance decreased slightly with the increase of annealing temperatures. The films were found to be crystalline having anatase phase. The refractive index of the films was found from 2.31-2.35 in the visible range. The extinction coefficient was nearly zero in the visible range and was found to increase with annealing temperature. The allowed indirect optical band gap of the films was estimated to be in the range from 3.39 to 3.42 eV which showed a small variation. The allowed direct band gap was found to increase from 3.67 to 3.72 eV. The porosity was also found to decrease at a higher annealing temperature making the film compact and dense.

Keywords: Titanium dioxide, RF reactive sputtering, Structuralproperties, Surface morphology, Optical properties.

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Authors: Pramod Jagtap, Kisan Jadhav, Neha Dand

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Risperidone (RISP) is an antipsychotic agent and has low water solubility and nontargeted delivery results in numerous side effects. Hence, an attempt was made to develop SLNs hydrogel for intranasal delivery of RISP to achieve maximum bioavailability and reduction of side effects. RISP loaded SLNs composed of 1.65% (w/v) lipid mass were produced by high shear homogenization (HSH) coupled ultrasound (US) method using glycerylmonostearate (GMS) or Imwitor 900K (solid lipid). The particles were loaded with 0.2% (w/v) of the RISP & surface-tailored with a 2.02% (w/v) non-ionic surfactant Tween® 80. Optimization was done using 32 factorial design using Design Expert® software. The prepared SLNs dispersion incorporated into Polycarbophil AA1 hydrogel (0.5% w/v). The final gel formulation was evaluated for entrapment efficiency, particle size, rheological properties, X ray diffraction, in vitro diffusion, ex vivo permeation using sheep nasal mucosa and histopathological studies for nasocilliary toxicity. The entrapment efficiency of optimized SLNs was found to be 76 ± 2%, polydispersity index <0.3., particle size 278 ± 5 nm. This optimized batch was incorporated into hydrogel. The pH was found to be 6.4 ± 0.14. The rheological behaviour of hydrogel formulation revealed no thixotropic behaviour. In histopathology study, there was no nasocilliary toxicity observed in nasal mucosa after ex vivo permeation. X-ray diffraction data shows drug was in amorphous form. Ex vivo permeation study shows controlled release profile of drug.

Keywords: Ex vivo, particle size, risperidone, solid lipid nanoparticles.

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Authors: Atef Y. Shenouda, Anton A. Momchilov

Abstract:

Graphene and CdO with different stoichiometric ratios of Cd(CH₃COO)₂ and graphene samples were prepared by hydrothermal reaction. The crystalline phases of pure CdO and 3CdO:1graphene were identified by X-ray diffraction (XRD). The particle morphology was studied with SEM. Furthermore, impedance measurements were applied. Galvanostatic measurements for the cells were carried out using potential limits between 0.01 and 3 V vs. Li/Li⁺. The current cycling intensity was 10⁻⁴ A. The specific discharge capacity of 3CdO-1G cell was about 450 Ah.Kg⁻¹ up to more than 100 cycles.

Keywords: CdO, graphene, negative electrode, lithium battery.

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Authors: O. Khalaj, B. Mašek, H. Jirková, J. Svoboda

Abstract:

By using a combination of new technologies together with an unconventional use of different types of materials, specific mechanical properties and structures of the material can be achieved. Some possibilities are enabled by a combination of powder metallurgy in the preparation of a metal matrix with dispersed stable particles achieved by mechanical alloying and hot consolidation. This paper explains the thermomechanical properties of new generation of Oxide Dispersion Strengthened alloys (ODS) within three ranges of temperature with specified deformation profiles. The results show that the mechanical properties of new ODS alloys are significantly affected by the thermomechanical treatment.

Keywords: Hot forming, ODS, alloys, thermomechanical, Fe-Al, Al2O3.

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Authors: O. Shiman, V. Gerbreders, E. Sledevskis, A. Bulanovs, V.Pashkevich

Abstract:

The selective wet-etching of amorphous and crystalline region of Sb20Se80 thin films was carried out using organic based solution e.g. amines. We report the development of an in situ real-time method to study the wet chemical etching process of thin films. Characterization of the structure and surface of films studied by X-ray diffraction, SEM and EBSD methods has been done and potential application suggested.

Keywords: amorphous and crystalline phases, chalcogenide thinfilm, etching process

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Authors: J. Hassan

Abstract:

Water 2H NMR signal on the surface of nano-silica material, MCM-41, consists of two overlapping resonances. The 2H water spectrum shows a superposition of a Lorentzian line shape and the familiar NMR powder pattern line shape, indicating the existence of two spin components. Chemical exchange occurs between these two groups. Decomposition of the two signals is a crucial starting point for study the exchange process. In this article we have determined these spin component populations along with other important parameters for the 2H water NMR signal over a temperature range between 223 K and 343 K.

Keywords: Nano-Silica, surface water, NMR

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Authors: Azam Anaraki Firooz, Ali Reza Mahjoub, Abbas Ali Khodadadi

Abstract:

The paper reports the preparation and photocatalytic activity of ZnO/SnO2 and SnO2 nanoparticles. These nanoparticles were synthesized by hydrothermal method. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Their grain sizes are about 50-100 nm. The photocatalytic activities of these materials were investigated for congo red removal from aqueous solution under UV light irradiation. It was shown that the use of ZnO/SnO2 as photocatalyst have better photocatalytic activity for degradation of congo red than SnO2 or TiO2 (anatase, particle size: 30nm) alone.

Keywords: ZnO/SnO2 nanoparticle, hydrothermal, photocatalysis

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

Abstract:

In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy, micro Raman spectroscopy, UV-Visible absorption spectroscopy, Photoluminescence spectroscopy, Field Effect Scanning Electron Microscopy.

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Authors: Peyman Moradi, Matin Parvari

Abstract:

Hydrodesulfurization (HDS) of dibenzothiophene (DBT) in a high pressure batch reactor was done at 320 °C on CoMoS/Al2O3-B2O3 (4, 10, and 16 wt. % of Boria) using nhexadecane as solvent, dimethyldisulfide (DMDS) in tetradecane as sulfur agent, and stirring at 1000 rpm. The effects of boria were investigated by using X-ray diffraction (XRD), Temperature programmed desorption (TPD) of ammonia, and Brunauer-Emmet- Teller (BET) experiments. The results showed that the catalyst prepared with low boria content (4 wt. %) had HDS activity (in pseudo first order kinetic constant basis) value ~1.45 times higher to that of CoMoS/Al2O3 catalyst.

Keywords: Alumina-boria mixed oxides, dibenzothiophene, hydrodesulfurization.

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Authors: Sabriye Piskin, Sibel Kasap, Muge Sari Yilmaz

Abstract:

Nanocrystalline TiO₂ particles were successfully synthesized via sol-gel and sonochemical combination using titanium tetraisopropoxide as a precursor at lower temperature for a short time. The effect of the reaction parameters (hydrolysis media, acid media, and reaction temperatures) on the synthesis of TiO₂ particles were investigated in the present study. Characterizations of synthesized samples were prepared by X-ray diffraction (XRD) analysis. It was shown that the reaction parameters played a significant role in the synthesis of TiO₂ particles.

Keywords: Crystalline TiO2, sonochemical mechanism, sol-gel reaction.

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Authors: M. Meskinfam , M. S. Sadjadi , H. Jazdarreh

Abstract:

In this study, synthesis of biomemitic patterned nano hydroxyapatite-starch biocomposites using different concentration of starch to evaluate effect of polymer alteration on biocomposites structural properties has been reported. Formation of hydroxyapatite nano particles was confirmed by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Size and morphology of the samples were characterized using scanning and transmission electron microscopy (SEM and TEM). It seems that by increasing starch content, the more active site of polymer (oxygen atoms) can be provided for interaction with Ca2+ followed by phosphate and hydroxyl group.

Keywords: Biocomposite, Biomimetic, Nano hydroxyapatite, Starch

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Authors: M. Jalali Azizpour, H. Mohammadi Majd

Abstract:

In this paper, the effect of WC-12Co particle velocity in HVOF thermal spraying process on the coating thickness has been studied. The statistical results show that the spray distance and oxygen-to-fuel ratio are more effective factors on particle characterization and thickness of HVOF thermal spraying coatings. Spray Watch diagnostic system, scanning electron microscopy (SEM), X-ray diffraction and thickness measuring system were used for this purpose.

Keywords: Grinding, HVOF, Thermal spray, WC-Co.

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Authors: Sh. Sohrabnezhad, A. Jafarzadeh

Abstract:

In this paper, MCM-41 mesoporous material nanofibers were synthesized by an electrospinning technique. The nanofibers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethyl orthosilicate (TEOS) and polyvinyl alcohol (PVA) were used as a silica source and fiber forming source, respectively. TEM and SEM images showed synthesis of MCM-41 nanofibers with a diameter of 200 nm. The pore diameter and surface area of calcined MCM-41 nanofibers was 2.2 nm and 970 m²/g, respectively. The morphology of the MCM-41 nanofibers depended on spinning voltages.

Keywords: Electrospinning, electron microscopy, fiber technology, porous materials, X-ray techniques.

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