Search results for: crystalline admixtures

Authors: Rym Sassi, Franck Fayon, Mohend Chaouche, Emmanuel Veron, Valerie Montouillout

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The chemical phenomena occurring during cement hydration are complex and interdependent, and even after almost two centuries of studies, they are still difficult to solve for complex mixtures combining different hydraulic binders. Powder-XRD has been widely used for characterizing the crystalline phases in both anhydrous and hydrated cement, but only limited information is obtained in the case of strongly disordered and amorphous phases. In contrast, local spectroscopies like solid-state NMR can provide a quantitative description of noncrystalline phases. In this work, the structural modifications occurring during hydration of a fast-setting ternary binder based on white Portland cement, white calcium aluminate cement, and calcium sulfate were investigated using advanced solid-state NMR methods. We particularly focused on the early stage of the hydration up to 28 days, working with samples whose hydration was controlled and stopped. ²⁷Al MQ-MAS as well as {¹H}-²⁷Al and {¹H}-²⁹Si Cross- Polarization MAS NMR techniques were combined to distinguish all of the aluminum and silicon species formed during the hydration. The NMR quantification of the different phases was conducted in parallel with the XRD analyses. The consumption of initial products, as well as the precipitation of hydraulic phases (ettringite, monosulfate, strätlingite, CSH, and CASH), were unambiguously quantified. Finally, the drawing of the consumption and formation of phases was correlated with mechanical strength measurements.

Keywords: cement, hydration, hydrates structure, mechanical strength, NMR

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Authors: Weeradej Cheewapattananuwong, Keeree Srivichian, Godchamon Somchai, Wasin Phusanong, Nontawat Yoddamnern

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Natural rubber used for traffic devices in Thailand has been developed and researched for several years. When compared with Dry Rubber Content (DRC), the quality of Rib Smoked Sheet (RSS) is better. However, the cost of admixtures, especially CaCO₃ and sulphur, is higher than the cost of RSS itself. In this research, Flexible Guideposts and Rubber Fender Barriers (RFB) are taken into consideration. In case of flexible guideposts, the materials used are both RSS and DRC60%, but for RFB, only RSS is used due to the controlled performance tests. The objective of flexible guideposts and RFB is to decrease a number of accidents, fatal rates, and serious injuries. Functions of both devices are to save road users and vehicles as well as to absorb impact forces from vehicles so as to decrease of serious road accidents. This leads to the mitigation methods to remedy the injury of motorists, form severity to moderate one. The solution is to find the best practice of traffic devices using natural rubber under the engineering concepts. In addition, the performances of materials, such as tensile strength and durability, are calculated for the modulus of elasticity and properties. In the laboratory, the simulation of crashes, finite element of materials, LRFD, and concrete technology methods are taken into account. After calculation, the trials' compositions of materials are mixed and tested in the laboratory. The tensile test, compressive test, and weathering or durability test are followed and based on ASTM. Furthermore, the Cycle-Repetition Test of Flexible Guideposts will be taken into consideration. The final decision is to fabricate all materials and have a real test section in the field. In RFB test, there will be 13 crash tests, 7 Pickup Truck tests, and 6 Motorcycle Tests. The test of vehicular crashes happens for the first time in Thailand, applying the trial and error methods; for example, the road crash test under the standard of NCHRP-TL3 (100 kph) is changed to the MASH 2016. This is owing to the fact that MASH 2016 is better than NCHRP in terms of speed, types, and weight of vehicles and the angle of crash. In the processes of MASH, Test Level 6 (TL-6), which is composed of 2,270 kg Pickup Truck, 100 kph, and 25 degree of crash-angle is selected. The final test for real crash will be done, and the whole system will be evaluated again in Korea. The researchers hope that the number of road accidents will decrease, and Thailand will be no more in the top tenth ranking of road accidents in the world.

Keywords: LRFD, load and resistance factor design, ASTM, american society for testing and materials, NCHRP, national cooperation highway research program, MASH, manual for assessing safety hardware

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Authors: S. Palaniyappan, P. K. Chennam, M. Trautmann, H. Ahmad, T. Mehner, T. Lampke, G. Wagner

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In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al₂O₃)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al₂O₃ respectively. Raman spectroscopic analyses produced no characteristic bands of Al₂O₃, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.

Keywords: Al₂O₃ thin film, electrical insulation coating, PVD process, SiC fibre, single fibre tensile test

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Authors: Meltem Bolluk, Ismail Duman

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Boron exhibits the properties of high melting temperature (2273K to 2573 K), high hardness (Mohs: 9,5), low density (2,340 g/cm3), high chemical resistance, high strength, and semiconductivity (band gap:1,6-2,1 eV). These superior properties enable to use it in several high-tech areas from electronics to nuclear industry and especially in high temperature metallurgy. Amorphous boron and crystalline boron have different application areas. Amorphous boron powder (directly amorphous and/or α-rhombohedral) is preferred in rocket firing, airbag inflating and in fabrication of superconducting MgB2 wires. The conventional ways to produce elemental boron with a purity of 85 pct to 95 prc are metallothermic reduction, fused salt electrolysis and mechanochemical synthesis; but the only way to produce high-purity boron powders is Chemical Vapour Deposition (Hot Surface CVD). In this study; amorphous boron powders with a minimum purity of 99,9 prc were synthesized in quartz tubes using BCl3-H2 gas mixture by CVD. Process conditions based on temperature and gas flow rate were determined. Thermodynamical interpretation of BCl3-H2 system for different temperatures and molar rates were performed using Fact Sage software. The characterization of powders was examined by using Xray diffraction (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM), Stereo Microscope (SM), Helium gas pycnometer analysis. The purities of final products were determined by titration after lime fusion.

Keywords: amorphous boron, CVD, powder production, powder characterization

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Authors: Maha Al-Ali, Selvakannan Periasamy, Rajarathinam Parthasarathy

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Drying temperature is an important factor impacting the physicochemical properties of the dried materials, particularly the pharmaceutical powders. Drying of pharmaceuticals by using microwave radiation is very limited, and the available information about the interaction between the electromagnetic radiations and the pharmaceutical material is still scarce. Therefore, microwave drying process is employed in this work to dry the wet (moisturised) granules of the formulated naproxen-sodium drug. This study aims to investigate the influences of the microwave radiation temperatures on the moisture removal, the crystalline structure, the size and morphology of the dried naproxen-sodium particles, and identify any potential changes in the chemical groups of the drug. In this work, newly formulated naproxen-sodium is prepared and moisturized by wet granulation process and hence dried by using microwave radiation at different temperatures. Moisture analyzer, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and scanning electron microscope are used to characterise the non-moisturised powder (reference powder), the moisturised granules, and the dried particles. The results show that microwave drying of naproxen-sodium at high drying temperature is more efficient than that at low temperatures in terms of the moisture removal. Although there is no significant change in the chemical structure of the dried particles, the particle size, crystallinity and morphology are relatively changed with changing of heating temperature.

Keywords: heating temperature, microwave drying, naproxen-sodium, particle size

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Authors: Srutirekha Giri, Manoranjan Sahoo, Anuradha Das, Pravanjan Mallick, Biswajit Mallick

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Ion Beam (IB) technique is a very powerful experimental technique for both material synthesis and material modifications. In this work, 3MeV proton beam was generated using the 3MV Tandem machine of the Institute of Physics, Bhubaneswar and extracted into air for the irradiation-induced modification purpose[1]. The polymeric material can be modeled for a three-phase system viz. crystalline(I), amorphous(II) and mesomorphic(III). So far, our knowledge is concerned. There are only few techniques reported for the synthesis of this third-phase(III) of polymer. The IB induced technique is one of them and has been reported very recently [2-4]. It was observed that by irradiating polyethylene terephthalate (PET) fiber at very low proton fluence, 10¹⁰ - 10¹² p/s, possess 2D mesophase structure. This was confirmed using X-ray diffraction technique. A low-intensity broad peak was observed at small angle of about 2θ =6º, when the fiber axis was mounted parallel to the X-ray direction. Such peak vanished in the diffraction spectrum when the fiber axis was mounted perpendicular to the beam direction. The appearance of this extra peak in a particular orientation confirms that the phase is 2-dimensionally oriented (mesophase). It is well known that the mesophase is a 2-dimensionally ordered structure but 3-dimensionally disordered. Again, the crystallite of the mesophase peak particle was measured about 3nm. The MeV proton-induced 2D mesophase patterning of nanocrystallites (3nm) of PET due to irradiation was observed within the above low fluence range and failed in high proton fluence. This is mainly due to the breaking of crystallites, radiation-induced thermal degradation, etc.

Keywords: Ion irradiation, mesophase, nanocrystallites, polymer

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Authors: Uchechukwu Vincent Okpala

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Under the Sun, energy is a key factor for the sustenance of life and its environment. The need to protect the environment as energy is generated and consumed has called for renewable and green energy sources. To be part of this green revolution, we synthesized and characterized undoped and velvet tamarind doped zinc sulfide (ZnS) crystals using sol-gel methods. Velvet tamarind was whittled down using the top-down approach of nanotechnology. Sodium silicate, tartaric acid, zinc nitrate, and thiourea were used as precursors. The grown samples were annealed at 105°C. Structural, optical, and compositional analyses of the grown samples revealed crystalline structures with varied crystallite sizes influenced by doping. Energy-dispersive X-ray spectroscopy confirmed elemental compositions of Zn, S, C and O in the films. Atomic percentages of the elements varied with VT doping. FT-IR analysis indicated the presence of functional groups like O-H stretching (alcohol), C=C=C stretching (alkene group), C=C bending, C-H stretching (alkane), N-H stretching (aliphatic primary amine) and N=C=S stretching (isothiocyanate) constituent in the film. The transmittance of the samples increased from the visible region to the infrared region making the samples good for poultry and solar energy applications. The bandgap energy of the films decreased as the number of VT drops increased, from 2.4 to 2.2. They were wide band gap materials and were good for optoelectronic, photo-thermal, high temperature, high power and solar cell applications.

Keywords: doping, sol-gel, velvet tamarind, ZnS.

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Authors: Muhammad Jawad Saleem, Faisal Hafeez, Muhammad Arshad, Afifa Naeem, Ayesha Iftekhar

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Bacillus thuringiensis is a gram-positive spore-forming bacterium that belongs to the Bacillus cereus group of Bacilli and it produces ICP (insecticidal crystal protein) Cry toxins or Cysts toxins. Spores are produced as parasporal crystalline inclusions bodies (also known as endotoxins) at the onset of sporulation during the stationary growth phase. During vegetative growth that does not form crystals and is called vegetative insecticidal proteins (VIP) and secreted an insecticidal protein (SIP). Bacillus thuringiensis (Bt) is important for pest management either in the form of insecticides or through incorporated in the gene of the crop. Bioassays were conducted on the F2 generation of 1st instar larvae of H. armigera by the diet incorporation method to determine the susceptibility to Bt Cry toxins (Cry1Ac, Cry2Ab, Cry2A). The median lethal concentration (LC₅₀) of Cry1Ac, Cry2Ab, Cry2A ranged from 0.11 to 1.06 µg/ml and moult inhibitory concentration (MIC₅₀) of Cry1Ac, Cry2Ab, Cry2A ranged from 0.05 to 0.25 µg/ml. Cry1Ac was found most toxic to 1st instar larvae of H. armigera as compared to other Bt Cry toxins (Cry1Ac, Cry2Ab, Cry2A). The experimental results are important to policy-makers and technology providers to develop strategies for the exploitation of transgenic Bt cotton varieties as a component of integrated pest management.

Keywords: Bt toxin, Cry1Ac, Cry2Ab, Cry2A, susceptibility, Helicoverpa armigera

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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: Erdem Elibol, Musa Cadırcı, Nedim Tutkun

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Recently, colloidal quantum dots (CQDs) have drawn increasing attention due to their unique size tunability, which makes them potential candidates for numerous applications including photovoltaic, LEDs, and imaging. However, the main challenge to exploit CQDs properly is that there has not been an effective method to produce them with highly crystalline form and narrow size dispersion. Hot injection method is one of the widely used techniques to produce high-quality nanoparticles. In this method, the key parameter is to reduce the time for injection of the precursors into each other, which yields fast and constant nucleation rate and hence to highly monodisperse QDs. In conventional hot injection method, the injection of precursors is carried out using standard lab syringes with long needles. However, this technique is relatively slow and thus will result in poor optical properties in QDs. In this work, highly luminescent CdTe QDs were synthesised by transferring hot precursors into each other using cannula method. Unlike regular syringe technique, with the help of high pressure difference between two precursors’ flasks and wide cross-section of cannula, the hot cannulation process is too short which yields narrow size distribution and high quantum yield of CdTe QDs. Here QDs with full width half maximum (FWHM) of 28 nm was achieved. In addition, the photoluminescence quantum yield of our samples was measured to be about 21 ± 0.9 which is at least twice the previous record values for CdTe QDs wherein syringe was used to transfer precursors.

Keywords: CdTe, hot injection method, luminescent, quantum dots

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Authors: Peter K. Galenko, Stefanie Koch, Markus Rettenmayr, Robert Wonneberger, Evgeny V. Kharanzhevskiy, Maria Zamoryanskaya, Vladimir Ankudinov

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We analyze the structure of undercooled melts, crystal growth kinetics and amorphous/crystalline microstructure of rapidly solidifying glass-forming Pd-based and CuZr-based alloys. A dendrite growth model is developed using a combination of the kinetic phase-field model and mesoscopic sharp interface model. The model predicts features of crystallization kinetics in alloys from thermodynamically controlled growth (governed by the Gibbs free energy change on solidification) to the kinetically limited regime (governed by atomic attachment-detachment processes at the solid/liquid interface). Comparing critical undercoolings observed in the crystallization kinetics with experimental data on melt viscosity, atomistic simulation's data on liquid microstructure and theoretically predicted dendrite growth velocity allows us to conclude that the dendrite growth kinetics strongly depends on the cluster structure changes of the melt. The obtained data of theoretical and experimental investigations are used for interpretation of microstructure of samples processed in electro-magnetic levitator on board International Space Station in the frame of the project "MULTIPHAS" (European Space Agency and German Aerospace Center, 50WM1941) and "KINETIKA" (ROSKOSMOS).

Keywords: dendrite, kinetics, model, solidification

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Authors: Dilip Depan, Austin Simoneaux, William Chirdon, Ahmed Khattab

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In this study, we present a novel approach to synthesize polymer nanocomposites with nanohybrid shish-kebab architecture (NHSK). For this low-density and high density polyethylene (PE) was crystallized on various carbon nano-fillers using a novel and convenient method to prepare high-yield NHSK. Polymer crystals grew epitaxially on carbon nano-fillers using a solution crystallization method. The mixture of polymer and carbon fillers in xylene was flocculated and precipitated in ethanol to improve the product yield. Carbon nanofillers of varying diameter were also used as a nucleating template for polymer crystallization. The morphology of the prepared nanocomposites was characterized scanning electron microscopy (SEM), while differential scanning calorimetry (DSC) was used to quantify the amount of crystalline polymer. Interestingly, whatever the diameter of the carbon nanofiller is, the lamellae of PE is always perpendicular to the long axis of nanofiller. Surface area analysis was performed using BET. Our results indicated that carbon nanofillers of varying diameter can be used to effectively nucleate the crystallization of polymer. The effect of molecular weight and concentration of the polymer was discussed on the basis of chain mobility and crystallization capability of the polymer matrix. Our work shows a facile, rapid, yet high-yield production method to form polymer nanocomposites to reveal application potential of NHSK architecture.

Keywords: carbon nanotubes, polyethylene, nanohybrid shish-kebab, crystallization, morphology

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Authors: S. Patel, T. Mitra, R. Dubey, J. Keller

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In the present investigations, an attempt has been made to study the charge storage mechanism and mechanism for the flow of transient charging and discharging current in an amorphous polymer (Polysulfone) (PSF) and a semi-crystalline polar Polyvinylidene fluoride (PVDF) blends in ratio PSF: PVDF: 80:20;85:15;90:10 and 95:05 at various poling temperatures (i.e. 60, 75, 90 and 1150C) and with field strength (100, 150, 200 and 250kVcm⁻¹). Thermally stimulated depolarizing current TSDC thermograms for (Polysulfone (PSF) and Polyvinylidene fluoride (PVDF) Blends sample have been obtained under different polarizing conditions. Peaks are found at high-temperature side. The variation of structure on blending and poling condition affects the magnitude of TSDC. The activation energy values have been calculated using the initial rise method of Garlick and Gibson. The transient current with the similar polarizing condition has been investigated over a period of 3X10³ sec. The observed characteristics obey Curie-Von Schweidler law in the studied temperature range. The charging current versus polarizing temperature curves at a constant time, i.e., isochronal current characteristics were studied and the activation energies were calculated. The activation energy in transient thermograms calculated by different methods is in good agreement with the values obtained from TSDC studies.

Keywords: activation energy, polysulfone (PSF), polyvinylidenefluoride (PVDF), thermally stimulated depolarizing current (TSDC)

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Authors: Collins C. Chiemeke, A. Onugba, P. Sule

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High resolution seismic reflection has recently been carried out on Zaria batholith, with the aim of characterizing the granitic Zaria batholiths in terms of its lithology. The geology of the area has revealed that the older granite outcrops in the vicinity of Zaria are exposures of a syntectonics to late-tectonic granite batholiths which intruded a crystalline gneissic basement during the Pan-African Orogeny. During the data acquisition the geophone were placed at interval of 1 m, variable offset of 1 and 10 m was used. The common midpoint (CMP) method with 12 fold coverage was employed for the survey. Analysis of the generated 3D surface of the p wave velocities from different profiles for densities and bulk modulus revealed that the rock material is more consolidated in South East part of the batholith and less consolidated in the North Western part. This was in conformity with earlier identified geology of the area, with the South Eastern part majorly of granitic outcrop, while the North Western part is characterized with the exposure of gneisses and thick overburden cover. The difference in lithology was also confirmed by the difference in seismic sections and Arial satellite photograph. Hence two major lithologies were identified, the granitic and gneisses complex which are characterized by gradational boundaries.

Keywords: basement complex, batholith, high resolution, lithologies, seismic reflection

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Authors: Jonathan Galvan-Colin, Ariel Valladares, Renela Valladares, Alexander Valladares

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Both porous materials and bulk metallic glasses have been studied due to their potential applications and their exceptional physical and chemical properties. However, each material presents certain drawbacks which have been thought to be overcome by generating bulk metallic glass foams (BMGF). Although some experimental reports have been performed on multicomponent BMGF, still no ab initio works have been published, as far as we know. We present an approach based on the expanding lattice (EL) method to generate binary amorphous nanoporous Cu64Zr36. Starting from two different configurations: a 108-atom crystalline cubic supercell (cCu64Zr36) and a 108-atom amorphous supercell (aCu64Zr36), both with an initial density of 8.06 g/cm3, we applied EL method to halve the density and to get 50% of porosity. After the lattice expansion the supercells were subject to ab initio molecular dynamics for 500 steps at constant room temperature. Then, the samples were geometry-optimized and characterized with the pair and radial distribution functions, bond-angle distributions and a coordination number analysis. We found that pores appeared along specific spatial directions different from one to another and that they differed in size and form as well, which we think is related to the initial structure. Due to the lack of experimental counterparts our results should be considered predictive and further studies are needed in order to handle a larger number of atoms and its implication on pore topology.

Keywords: ab initio molecular dynamics, bulk mettalic glass, porous alloy

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Authors: Rudra Vaghela, P. K. Kulkarni

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The aim of the present research was to develop oral Amphotericin B (AmB) nanocrystals (Nc) grafted with suitable ligand in order to enhance drug transport across the intestinal epithelial barrier and subsequently, active uptake by macrophages. AmB Nc were prepared by liquid anti-solvent precipitation technique (LAS). Poloxamer 188 was used to stabilize the prepared AmB Nc and grafted with mannose for actively targeting M cells in Peyer’s patches. To prevent shedding of the stabilizer and ligand, N,N’-Dicyclohexylcarbodiimide (DCC) was used as a cross-linker. The prepared AmB Nc were characterized for particle size, PDI, zeta potential, X-ray diffraction (XRD) and surface morphology using scanning electron microscope (SEM) and evaluated for drug content, in vitro drug release and cell uptake studies using caco-2 cells. The particle size of stabilized AmB Nc grafted with WGA was in the range of 287-417 nm with negative zeta potential between -18 to -25 mV. XRD studies revealed crystalline nature of AmB Nc. SEM studies revealed that ungrafted AmB Nc were irregular in shape with rough surface whereas, grafted AmB Nc were found to be rod-shaped with smooth surface. In vitro drug release of AmB Nc was found to be 86% at the end of one hour. Cellular studies revealed higher invasion and uptake of AmB Nc towards caco-2 cell membrane when compared to ungrafted AmB Nc. Our findings emphasize scope on developing oral delivery system for passively targeting M cells in Peyer’s patches.

Keywords: leishmaniasis, amphotericin b nanocrystals, macrophage targeting, LAS technique

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Authors: Schirin Hanf, Carlos Lizandara-Pueyo, Timmo P. Emmert, Ivana Jevtovikj, Roger Gläser, Stephan A. Schunk

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Metal alkoxides are very versatile precursors for a broad array of complex functional materials. However, metal alkoxides, especially transition metal alkoxides, tend to form oligomeric structures due to the very strong M–O–M binding motif. This fact hinders their facile application in sol-gel-processes and complicates access to complex carbonate or oxidic compounds after hydrolysis of the precursors. Therefore, the development of a synthetic alternative with the aim to grant access to carbonates and hydroxycarbonates from simple metal alkoxide precursors via hydrolysis is key to this project. Our approach involves the reaction of metal alkoxides with unsaturated isoelectronic molecules, such as carbon dioxide. Subsequently, a stoichiometric insertion of the CO₂ into the alkoxide M–O bond takes place and leads to the formation of soluble metal alkyl carbonates. This strategy is a very elegant approach to solubilize metal alkoxide precursors to make them accessible for sol-gel chemistry. After hydrolysis of the metal alkyl carbonates, crystalline metal carbonates, and hydroxycarbonates can be obtained, which were then utilized for the synthesis of Cu/Zn based bulk catalysts for methanol synthesis. Using these catalysts, a comparable catalytic activity to commercially available MeOH catalysts could be reached. Based on these results, a complement for traditional precipitation techniques, which are usually utilized for the synthesis of bulk methanol catalysts, have been found based on an alternative solubilization strategy.

Keywords: metal alkoxides, metal carbonates, metal hydroxycarbonates, CO₂ insertion, solubilization

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Authors: Bastola Narayan, Rajeev Ranjan

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The morphotropic phase boundary (MPB) in the magnetoelectric (1-x)BiFeO3-(x)PbTiO3 has remained a matter of controversy ever since its discovery in 1964. The nature of the phase stabilized (single phase tetragonal or coexistence of tetragonal and rhombohedral phases) is very sensitive to the slight changes in the synthesis conditions. It thus remained an enigma as to what is the essential physical factor which is controlled by the slight difference in the synthesis conditions that finally determines, whether the phase formed will be single phase or coexistence of phases. In this paper, we demonstrate that the nature of the phase stabilized in this system is uniquely dependent on the crystallite size. The system is shown to exhibit features of abnormal grain growth (AGG) during sintering with abrupt increase in the grain size from ~ 1 micron to ~ 10 microns. The 10 micron grains exhibit pure tetragonal phase while the 1 micron grains exhibit coexistence of rhombohedral and tetragonal ferroelectric phases. The Rietveld analysis of powder neutron diffraction shows a paramagnetic to antiferromagnetic order transition inducing with crystalline size reduction from 10 micron to 1 micron. Since tetragonal phase is known to have paramagnetic order and rhombohedral phase has antiferromagnetic order in room temperature, this further strengthens our argument of size induced structure transition.

Keywords: size driven MPB, size driven magnetic ordering, abnormal grain growth, phase formation in BF-PT system

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Authors: Darlington Ashiegbu, Herman Johannes Potgieter

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The increasing utilization of Zinc Oxide (ZnO) as a better alternative to TiO₂ has been attributed to its wide bandgap (3.37eV), lower production cost, ability to absorb over a larger range of the UV-spectrum and higher efficiency in some cases. ZnO nanoparticles were synthesized via sol-gel process and calcined at 400ᵒC, 500ᵒC, and 650ᵒC. The as-synthesized nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and Brunauer–Emmett–Teller (BET) surface area measurement. Scanning electron micrograph revealed pseudo-spherical and rod-like morphologies and a high rate of agglomeration for the sample calcined at 650ᵒC, Brunnauer Emmett Teller (BET) surface area measurement was highest in the sample calcined at 500ᵒC, energy dispersive X-ray spectroscopy (EDS) results confirmed the purity of the samples as only Zn and O₂ were detected and X-ray diffraction (XRD) results revealed crystalline hexagonal wurtzite structure of the ZnO nanoparticles. All three samples were utilized in the degradation of ethylbenzene, and a UV-Vis spectrophotometer was utilized in monitoring degradation of ethylbenzene. The sample calcined at 500ᵒC had the highest surface area for reaction, lowest agglomeration and the highest photocatalytic activity in the degradation of ethylbenzene. This revealed temperature as a very important factor in improved and higher photocatalytic activity.

Keywords: ethylbenzene, pseudo-spherical, sol-gel, zinc oxide

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Authors: Kkochorong Park, Keun Cheon Kim, Hyoban Lee, Eun Ju Lee, Bongsoo Kim

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Introduction of biomaterials such as DNA, RNA, proteins is important for many research areas. There are many methods to introduce biomaterials into living organisms like tissue and cells. To introduce biomaterials, several indirect methods including virus‐mediated delivery, chemical reagent (i.e., lipofectamine), electrophoresis have been used. Such methods are passive delivery using an endocytosis process of cell, reducing an efficiency of delivery. Unlike the indirect delivery method, it has been reported that a direct delivery of exogenous biomolecules into nucleus have been more efficient to expression or integration of biomolecules. Nano-sized material is beneficial for detect signal from cell or deliver stimuli/materials into the cell at cellular and molecular levels, due to its similar physical scale. Especially, because 1 dimensional (1D) nanomaterials such as nanotube, nanorod and nanowire with high‐aspect ratio have nanoscale geometry and excellent mechanical, electrical, and chemical properties, they could play an important role in molecular and cellular biology. In this study, by using single crystalline 1D noble metal nanowire, we fabricated nano-sized 1D injector which can successfully interface with living cells and directly deliver biomolecules into several types of cell line (i.e., stem cell, mammalian embryo) without inducing detrimental damages on living cell. This nano-bio technology could be a promising and robust tool for introducing exogenous biomaterials into living organism.

Keywords: DNA, gene delivery, nanoinjector, nanowire

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Authors: Oshada Gamage, Chamal Wimalasooriya, Chrismal Boteju, W. K. Wimalsiri

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This paper presents a study on the feasibility of introducing a solar powered propelling mechanism to multi-day fishing boats as an alternative energy source. Since solar energy is readily available on the sea throughout the year, this free energy could be utilized to power multi-day fishing vessels. Multi-day boats have a large deck area where solar panels can be mounted above without much effort. This project involves studying the amount of power that can be generated using onboard solar panels and implementing an independent propelling system to run the boat. A chain drive system was designed to propel the boat, when the batteries are fully charged, from an electric motor using the same propeller. A 60 feet multi-day fishing boat built by a local boat manufacturer was chosen for the study. The service speed of the boat was around 6 knots with the electric motor, and the duration of cruising is 1 hour per day with around 11 hours of charging. 350-watt Mono-crystalline PV module, 75 kW HVH type motor, and 10 kWh lithium-ion battery packs were chosen for the study. From the calculations, it was obtained that the boat has 30 PV modules (10.5 kW), 5 batteries (47 kWh), The boat dimensions are 20 meter length of water line, 5.51 meter of beam, 1.8 meter of draught, and 77 ton of total displacement with the PV system net present value of USD 12445 for 20 years of operation and a payback period of around 8.2 years.

Keywords: multiday fishing boats, photovoltaic cells, solar energy, solar powered boat

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Authors: Sirirat Jangkorn, Pornsawai Praipipat

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Sugarcane bagasse ash of sugar factories is solid wastes that the richest source of silica. The alkali fusion method, quartz particles in material can be dissolved and they can be used as the silicon source for synthesizing silica-based materials such as zeolites. Zeolites have many advantages such as catalyst to improve the chemical reactions and they can also remove heavy metals in the water including lead. Therefore, this study attempts to synthesize zeolites from the sugarcane bagasse ash, investigate their structure characterizations and chemical components to confirm the happening of zeolites, and examine their lead removal efficiency through the batch test studies. In this study, the sugarcane bagasse ash was chosen as the silicon source to synthesize zeolites, X-ray diffraction (XRD) and X-ray fluorescence spectrometry (XRF) were used to verify the zeolite pattern structures and element compositions, respectively. The batch test studies in dose (0.05, 0.1, 0.15 g.), contact time (1, 2, 3), and pH (3, 5, 7) were used to investigate the lead removal efficiency by the synthesized zeolite. XRD analysis result showed the crystalline phase of zeolite pattern, and XRF result showed the main element compositions of the synthesized zeolite that were SiO₂ (50%) and Al₂O₃ (30%). The batch test results showed the best optimum conditions of the synthesized zeolite for lead removal were 0.1 g, 2 hrs., and 5 of dose, contact time, and pH, respectively. As a result, this study can conclude that the zeolites can synthesize from the sugarcane bagasse ash and they can remove lead in the water.

Keywords: sugarcane bagasse ash, solid wastes, zeolite, lead

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Authors: Carolin Lutz, Jörg Matthes, Patrick Waibel, Ulrich Precht, Krassimir Garbev, Günter Beuchle, Uwe Schweike, Peter Stemmermann, Hubert B. Keller

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Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Keywords: calibration model, celitement, cementitious material, NIR spectroscopy

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Authors: Anton S. Perin, Vladimir M. Shandarov

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Compensation for the nonlinear diffraction of narrow laser beams with wavelength of 532 and the formation of photonic waveguides and waveguide circuits due to the contribution of pyroelectric effect to the nonlinear response of lithium niobate crystal have been experimentally demonstrated. Complete compensation for the linear and nonlinear diffraction broadening of light beams is obtained upon uniform heating of an undoped sample from room temperature to 55 degrees Celsius. An analysis of the light-field distribution patterns and the corresponding intensity distribution profiles allowed us to estimate the spacing for the channel waveguides. The observed behavior of bright soliton beams may be caused by their coherent interaction, which manifests itself in repulsion for anti-phase light fields and in attraction for in-phase light fields. The experimental results of this study showed a fundamental possibility of forming optically complex waveguide structures in lithium niobate crystals with pyroelectric mechanism of nonlinear response. The topology of these structures is determined by the light field distribution on the input face of crystalline sample. The optical induction of channel waveguide elements by interacting spatial solitons makes it possible to design optical systems with a more complex topology and a possibility of their dynamic reconfiguration.

Keywords: self-action, soliton, lithium niobate, piroliton, photorefractive effect, pyroelectric effect

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

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

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

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Authors: Eman A. Alghamdi, A. M. Aldhafiri

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It was found that the induce an isolated dopant close to the middle of the bandgap by occupying the Cd position in the CdTe lattice structure is an efficient factor in reducing the nonradiative recombination rate and increasing the solar efficiency. According to our laboratory results, this work has been carried out to obtain the effect of substrate temperature on the CdTe0.6Sn0.4 prepared by thermal evaporation technique for photovoltaic application. Various substrate temperature (25°C, 100°C, 150°C, 200°C, 250°C and 300°C) was applied. Sn-doped CdTe thin films on a glass substrate at a different substrate temperature were made using CdTe and SnTe powders by the thermal evaporation technique. The structural properties of the prepared samples were determined using Raman, x-Ray Diffraction. Spectroscopic ellipsometry and spectrophotometric measurements were conducted to extract the optical constants as a function of substrate temperature. The structural properties of the grown films show hexagonal and cubic mixed structures and phase change has been reported. Scanning electron microscopy (SEM) reviled that a homogenous with a bigger grain size was obtained at 250°C substrate temperature. The conductivity measurements were recorded as a function of substrate temperatures. The open-circuit voltage was improved by controlling the substrate temperature due to the improvement of the fundamental material issues such as recombination and low carrier concentration. All the result was explained and discussed on the biases of the influences of the Sn dopant and the substrate temperature on the structural, optical and photovoltaic characteristics.

Keywords: CdTe, conductivity, photovoltaic, ellipsometry

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Authors: Akshita Jindal, Renu Chadha, Maninder Karan

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Supramolecular chemistry has gained recent eminence in a flurry of research documents demonstrating the formation of new crystalline forms with potentially advantageous characteristics. Mesalamine (5-amino salicylic acid) belongs to anti-inflammatory class of drugs, is used to treat ulcerative colitis and Crohn’s disease. Unfortunately, mesalamine suffer from poor solubility and therefore very low bioavailability. This work is focused on preparation and characterization of cocrystal of mesalamine with nicotinamide (MNIC) a coformer of GRAS status. Cocrystallisation was achieved by solvent drop grinding in stoichiometric ratio of 1:1 using acetonitrile as solvent and was characterized by various techniques including DSC (Differential Scanning Calorimetry), PXRD (X-ray Powder Diffraction), and FTIR (Fourier Transform Infrared Spectrometer). The co-crystal depicted single endothermic transitions (254°C) which were different from the melting peaks of both drug (288°C) and coformer (128°C) indicating the formation of a new solid phase. Different XRPD patterns and FTIR spectrums for the co-crystals from those of individual components confirms the formation of new phase. Enhancement in apparent solubility study and intrinsic dissolution study showed effectiveness of this cocrystal. Further improvement in pharmacokinetic profile has also been observed with 2 folds increase in bioavailability. To conclude, our results show that application of nicotinamide as a coformer is a viable approach towards the preparation of cocrystals of potential drug molecule having limited solubility.

Keywords: cocrystal, mesalamine, nicotinamide, solvent drop grinding

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Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks

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Surface enhanced Raman spectroscopy (SERS) of Silicon nano crystals (SiNCs) were obtained using two different laser excitations: 488 nm and 514.5 nm. Silver nano particles were used as plasmonics metal nano particles due to a robust SERS effect that observed when they mixed with SiNCs. SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. Silver nano particles (AgNPs) of two different sizes were synthesized using photo chemical reduction of AgNO3 with sodium dodecyl sulfate (SDS). The synthesized AgNPs have a polycrystalline structure with an average particle diameter of 100 nm and 30 nm, respectively. A significant enhancement in the SERS intensity was observed for AgNPs100/SiNCs and AgNPs30/SiNCs mixtures increasing up to 9 and 3 times respectively using 488 nm intensity; whereas the intensity of the SERS signal increased up to 7 and 2 times respectively, using 514.5 nm excitation source. The enhancement in SERS intensities occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs. The results provide good consensus between the wavelength of the laser excitation source and surface plasmon resonance absorption band of silver nano particles consider to be an important requirement in SERS experiments.

Keywords: silicon nanocrystals (SiNCs), silver nanoparticles (AgNPs), surface enhanced raman spectroscopy (SERS)

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Authors: Zehui Du, Chaiwat Prapainainar, Paisan Kongkachuichay, Paweena Prapainainar

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The aim of this work was to obtain small crystalline size and high crystallinity of mordenites and analcimes, by modifying the aging time, agitation, water content, crystallization temperature and crystallization time. Two different hydrothermal methods were studied. Both methods used Na2SiO3 as the silica source, NaAlO2 as the aluminum source, and NaOH as the alkali source. The first method used HMI as the template while the second method did not use the template. Mordenite crystals with spherical shape and bimodal in size of about 1 and 5 µm were obtained from the first method using conditions of 24 hr aging time, 170°C and 24 hr crystallization. Modernites with high crystallinity were formed using agitation system in the crystallization process. It was also found that the aging time of 2 hr and 24 hr did not much affect the formation of mordenite crystals. Analcime crystals were formed in spherical shape and facet on surface with the size between 13-15 µm by the second method using the conditions of 30 minutes aging time, 170°C and 24 hr crystallization without calcination. By increasing water content, the crystallization process was slowed down and resulted in smaller analcime crystals. Larger size of analcime crystals were observed when the samples were calcined at 300°C and 580°C. Higher calcination temperature led to higher crystal growth and resulted in larger crystal size. Finally, mordenite and analcime was used as fillers in zeolite/Nafion composite membrane to solve the fuel cross over problem in direct alcohol fuel cell.

Keywords: analcime, hydrothermal synthesis, mordenite, zeolite

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Authors: Harshada Vaidya-Kannur, Dattatraya Naik

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Propolis, one of the beehive products also referred as bee-glue is sticky dark coloured complex mixture of compounds. The volatile oil can be isolated from the propolis by hydrodistillation. The mark that is left behind after the removal of volatile oil is referred as the de-oiled propolis. Antioxidant as well as anti-inflammatory properties of total ethanolic extract of de-oiled propolis (TEEDP) was investigated. Another lot of deoiled propolis was successively exacted with hexane, ethyl acetate and ethanol. Activities of these fractions were also determined. Antioxidant activity was determined by studying ABTS, DPPH and NO radical scavenging. Determination of anti-inflammatory activity was carried out by topical TPA induced mouse ear oedema model. It is noteworthy that ethyl acetate fraction of deoiled propolis (EAFDP) exhibited 49.45 % TEAC activity at the concentration 0.2 mg/ml which is equivalent to the activity of trolox at the concentration 0.2 mg/ml. Its DPPH scavenging activity (72.56%) was closely comparable to that of trolox (75%). However its NO scavenging activity was comparatively low. From IC50 values it could be concluded that the efficiency of scavenging ABTS radicals by the de-oiled propolis was more pronounced as compared to scavenging of other radicals. Studies by TPA induced mouse ear inflammation model indicated that the de-oiled propolis of Indian origin had significant topical anti-inflammatory activity. The EAFDP was found to be the most active fraction for this activity also. The purification of EAFP yielded six pure crystalline compounds. These compounds were identified by their physical data and spectral data.

Keywords: anti-inflammatory activity, anti-oxidant activity, column chromatography, de-oiled propolis

Procedia PDF Downloads 267