Search results for: nanocrystalline powders

Authors: Umashankar Morya, Somnath Basu

Abstract:

Metalloids like arsenic are often present as contaminants in industrial effluents. Removal of the same is essential before the safe discharge of the wastewater into the environment. Otherwise, these pollutants tend to percolate into aquifers over a period of time and contaminate drinking water sources. Several adsorbents, including metal powders, carbon nanotubes and zeolites, are being used for this purpose, with varying degrees of success. However, most of these solutions are not only costly but also not always readily available. This restricts their use, especially among financially weaker communities. Slag generated globally from primary steelmaking operations exceeds 200 billion kg every year. Some of it is utilized for applications like road construction, filler in reinforced concrete, railway track ballast and recycled into iron ore agglomeration processes. However, these usually involve low-value addition, and a significant amount of the slag still ends up in a landfill. However, there is a strong possibility that the constituents in the steelmaking slag may immobilize metalloid contaminants present in wastewater through a combination of adsorption and precipitation of insoluble product(s). Preliminary experiments have already indicated that exposure to basic oxygen steelmaking slag does reduce pollutant concentration in wastewater. In addition, the slag is relatively inexpensive and available in large quantities and in several countries across the world. Investigations on the mechanism of interactions at the water-solid interfaces have been in progress for some time. However, at the same time, there are concerns about the possibility of leaching of metal ions from the slag particles in concentrations greater than what exists in the water bodies where the “treated” wastewater would eventually be discharged. The effect of such leached ions on the aquatic flora and fauna is yet uncertain. This has prompted the present investigation, which focuses on the leaching of metal ions from steelmaking slag particles in contact with wastewater, and the influence of these ions on the removal of contaminant species. Experiments were carried out to quantify the leaching behavior of different ionic species upon exposure of the slag particles to simulated wastewater, both with and without specific metalloid contaminants.

Keywords: slag, water, metalloid, heavy metal, wastewater

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Authors: A. Saravanan, B. R. Huang, C. J. Yeh, K. C. Leou, I. N. Lin

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A new class of ultra-nano diamond-graphite nano-hybrid (DGH) composite materials containing nano-sized diamond needles was developed at low temperature process. Such kind of diamond- graphite nano-hybrid composite nanowires exhibit high electrical conductivity and excellent electron field emission (EFE) properties. Few earlier reports mention that addition of N2 gas to the growth plasma requires high growth temperature (800°C) to trigger the dopants to generate the conductivity in the films. High growth temperature is not familiar with the Si-based device fabrications. We have used a novel process such as bias-enhanced-grown (beg) MPECVD process to grow diamond films at low substrate temperature (450°C). We observed that the beg-N/UNCD films thus obtained possess high conductivity of σ=987 S/cm, ever reported for diamond films with excellent Electron field emission (EFE) properties. TEM investigation indicated that these films contain needle-like diamond grains about 5 nm in diameter and hundreds of nanometers in length. Each of the grains was encased in graphitic layers about tens of nano-meters in thickness. These materials properties suitable for more specific applications, such as high conductivity for electron field emitters, high robustness for microplasma cathodes and high electrochemical activity for electro-chemical sensing. Subsequently, other hand, the highly conducting DGH films were coated on vertically aligned ZnO nanorods, there is no prior nucleation or seeding process needed due to the use of BEG method. Such a composite structure provides significant enhancement in the field emission characteristics of the cold cathode was observed with ultralow turn on voltage 1.78 V/μm with high EFE current density of 3.68 mA/ cm2 (at 4.06V/μm) due to decoration of DGH material on ZnO nanorods. The DGH/ZNRs based device get stable emission for longer duration of 562min than bare ZNRs (104min) without any current degradation because the diamond coating protects the ZNRs from ion bombardment when they are used as the cathode for microplasma devices. The potential application of these materials is demonstrated by the plasma illumination measurements that ignited the plasma at the minimum voltage by 290 V. The photoresponse (Iphoto/Idark) behavior of the DGH/ZNRs based photodetectors exhibits a much higher photoresponse (1202) than bare ZNRs (229). During the process the electron transport is easy from ZNRs to DGH through graphitic layers, the EFE properties of these materials comparable to other primarily used field emitters like carbon nanotubes, graphene. The DGH/ZNRs composite also providing a possibility of their use in flat panel, microplasma and vacuum microelectronic devices.

Keywords: bias-enhanced nucleation and growth, ZnO nanorods, electrical conductivity, electron field emission, photo-detectors

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Authors: Sarah Nasser, Anne Moreau, Alain Hedoux, Romain Jeantet, Guillaume Delaplace

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Background: Spray dryed powders containing some caseins are commonly produced in dairy industry. It is widely admitted that the structure of casein evolves during powder storage, inducing a loss of solubility. However few studies evaluate accurately the destabilization mechanisms at molecular and mesoscopic level, in particular for Native Phospho Casein powder (NPC). Consequently, at the state of the art, it is very difficult to assess which secondary structure change or crosslinks initiate insolubility during storage. To address this issue, controlled ageing conditions have been applied to a NPC powder (which was obtained by spray drying a concentrate containing a higher content of casein (90%), whey protein (8%) and lactose (few %)). Evolution of structure and loss of solubility, with the effects of temperature and time of storage were systematically reported. Methods: FTIR spectroscopy, Raman and Circular Dichroism were used to monitor changes of secondary structure in dry powder and in solution after rehydration. Besides, proteomic tools and electrophoresis have been performed after varying storage conditions for evaluating aggregation and post translational modifications, like lactosylation or phosphorylation. Finally, Tof Sims and MEB were used to follow in parallel evolution of structure in surface and skin formation due to storage. Results + conclusion: These results highlight the important role of storage temperature in the stability of NPC. It is shown that this is not lactosylation at the heart of formation of aggregates, as advanced in others publications This is almost the rise of multitude post translational modifications (chemical cross link), added to disulphide bridges (physical cross link) wich contribute to the destabilisation of structure and aggregation of casein. A relative quantification of each kind of cross link, source of aggregates, is proposed. In addition, it has been proved that migration of lipids and formation of skin in surface during the ageing also explains the evolution of structure casein and thus the alterations of functional properties of NPC powder.

Keywords: casein, cross link, powder, storage

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Authors: Farha Mizana Shamsudin, Shahidan Radiman, Yusof Abdullah, Nasri Abdul Hamid

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Oxide dispersion strengthened (ODS) ferritic steels are amongst the most promising candidates for large scale structural materials to be applied in next generation fission and fusion nuclear power reactors. This kind of material is relatively stable at high temperature, possess remarkable mechanical properties and comparatively good resistance from neutron radiation damage. The superior performance of ODS ferritic steels over their conventional properties is attributed to the high number density of nano-sized dispersoids that act as nucleation sites and stable sinks for many small helium bubbles resulting from irradiation, and also as pinning points to dislocation movement and grain growth. ODS ferritic steels are usually produced by powder metallurgical routes involving mechanical alloying (MA) process of Y2O3 and pre-alloyed or elemental metallic powders, and then consolidated by hot isostatic pressing (HIP) or hot extrusion (HE) techniques. In this study, Fe-14Cr-3W-0.5Ti-0.3Y₂O₃ (designated as 14YWT) was produced by mechanical alloying process and followed by hot isostatic pressing (HIP) technique. Crystal structure and morphology of this sample were identified and characterized by using X-ray Diffraction (XRD) and field emission scanning electron microscope (FESEM) respectively. The magnetic measurement of this sample at room temperature was carried out by using a vibrating sample magnetometer (VSM). FESEM micrograph revealed a homogeneous microstructure constituted by fine grains of less than 650 nm in size. The ultra-fine dispersoids of size between 5 nm to 19 nm were observed homogeneously distributed within the BCC matrix. The EDS mapping reveals that the dispersoids contain Y-Ti-O nanoclusters and from the magnetization curve plotted by VSM, this sample approaches the behavior of soft ferromagnetic materials. In conclusion, ODS Fe-14Cr-3W-0.5Ti-0.3Y₂O₃ (14YWT) ferritic steel was successfully produced by HIP technique in this present study.

Keywords: hot isostatic pressing, magnetization, microstructure, ODS ferritic steel

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Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

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The process of assembling metal nanoparticles at the interface of two liquids has received a great interest over the past few years due to a wide range of important applications and their unusual properties compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: firstly, to describe the achievement of a closed loop recycling for producing cadmium sulphide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulphides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be applied to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferro-fluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Noble metal like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: assembling nanoparticles, liquid/liquid interface, thin film, core/shell, solar cells, recording media

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Authors: Bijit Kalita, R. Jayaganthan

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Additive manufacturing (AM) is a novel manufacturing method which provides more freedom in design, manufacturing near-net-shaped parts as per demand, lower cost of production, and expedition in delivery time to market. Among various metals, AM techniques, Laser Powder Bed Fusion (L-PBF) is the most prominent one that provides higher accuracy and powder proficiency in comparison to other methods. Particularly, 17-4 PH alloy is martensitic precipitation hardened (PH) stainless steel characterized by resistance to corrosion up to 300°C and tailorable strengthening by copper precipitates. Additively manufactured 17-4 PH stainless steel exhibited a dendritic/cellular solidification microstructure in the as-built condition. It is widely used as a structural material in marine environments, power plants, aerospace, and chemical industries. The excellent weldability of 17-4 PH stainless steel and its ability to be heat treated to improve mechanical properties make it a good material choice for L-PBF. In this study, the microstructures of martensitic stainless steels in the as-built state, as well as the effects of process parameters, building atmosphere, and heat treatments on the microstructures, are reviewed. Mechanical properties of fabricated parts are studied through micro-hardness and tensile tests. Tensile tests are carried out under different strain rates at room temperature. In addition, the effect of process parameters and heat treatment conditions on mechanical properties is critically reviewed. These studies revealed the performance of L-PBF fabricated 17–4 PH stainless-steel parts under cyclic loading, and the results indicated that fatigue properties were more sensitive to the defects generated by L-PBF (e.g., porosity, microcracks), leading to the low fracture strains and stresses under cyclic loading. Rapid melting, solidification, and re-melting of powders during the process and different combinations of processing parameters result in a complex thermal history and heterogeneous microstructure and are necessary to better control the microstructures and properties of L-PBF PH stainless steels through high-efficiency and low-cost heat treatments.

Keywords: 17–4 PH stainless steel, laser powder bed fusion, selective laser melting, microstructure, additive manufacturing

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Authors: Laura Kocsor, Laszlo Peter, Laszlo Kovacs, Zsolt Kis

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The aim of our research is to prepare rare-earth-doped lithium niobate (LiNbO3) nanocrystals, having only a few dopant ions in the focal point of an exciting laser beam. These samples will be used to achieve individual addressing of the dopant ions by light beams in a confocal microscope setup. One method for the preparation of nanocrystalline materials is to reduce the particle size by mechanical grinding. High-energy ball-milling was used in several works to produce nano lithium niobate. Previously, it was reported that dry high-energy ball-milling of lithium niobate in a shaker mill results in the partial reduction of the material, which leads to a balanced formation of bipolarons and polarons yielding gray color together with oxygen release and Li2O segregation on the open surfaces. In the present work we focus on preparing LiNbO3 nanocrystals by high-energy ball-milling using a Fritsch Pulverisette 7 planetary mill. Every ball-milling process was carried out in zirconia vial with zirconia balls of different sizes (from 3 mm to 0.1 mm), wet grinding with water, and the grinding time being less than an hour. Gradually decreasing the ball size to 0.1 mm, an average particle size of about 10 nm could be obtained determined by dynamic light scattering and verified by scanning electron microscopy. High-energy ball-milling resulted in sample darkening evidenced by optical absorption spectroscopy measurements indicating that the material underwent partial reduction. The unwanted lithium oxide loss decreases the Li/Nb ratio in the crystal, strongly influencing the spectroscopic properties of lithium niobate. Zirconia contamination was found in ground samples proved by energy-dispersive X-ray spectroscopy measurements; however, it cannot be explained based on the hardness properties of the materials involved in the ball-milling process. It can be understood taking into account the presence of lithium hydroxide formed the segregated lithium oxide and water during the ball-milling process, through chemically induced abrasion. The quantity of the segregated Li2O was measured by coulometric titration. During the wet milling process in the planetary mill, it was found that the lithium oxide loss increases linearly in the early phase of the milling process, then a saturation of the Li2O loss can be seen. This change goes along with the disappearance of the relatively large particles until a relatively narrow size distribution is achieved in accord with the dynamic light scattering measurements. With the 3 mm ball size and 1100 rpm rotation rate, the mean particle size achieved is 100 nm, and the total Li2O loss is about 1.2 wt.% of the original LiNbO3. Further investigations have been done to minimize the Li2O segregation during the ball-milling process. Since the Li2O loss was observed to increase with the growing total surface of the particles, the influence of ball-milling parameters on its quantity has also been studied.

Keywords: high-energy ball-milling, lithium niobate, mechanochemical reaction, nanocrystals

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Authors: Vishal Mahale, Jayashree Bijwe, Sujeet K. Sinha

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Range of thermal conductivity (TC) of Friction Materials (FMs) is a critical issue since lower TC leads to accumulation of frictional heat on the working surface, which results in excessive fade while higher TC leads to excessive heat flow towards back-plate resulting in boiling of brake-fluid leading to ‘spongy brakes’. This phenomenon prohibits braking action, which is most undesirable. Therefore, TC of the FMs across the brake pads should not be high while along the brake pad, it should be high. To enhance TC, metals in the forms of powder and fibers are used in the FMs. Apart from TC improvement, metals provide strength and structural integrity to the composites. Due to higher TC Copper (Cu) powder/fiber is a most preferred metallic ingredient in FM industry. However, Cu powders/fibers are responsible for metallic wear debris generation, which has harmful effects on aquatic organisms. Hence to get rid of a problem of metallic wear debris generation and to keep the positive effect of TC improvement, incorporation of Cu fabric in NAO brake-pads can be an innovative solution. Keeping this in view, two realistic multi-ingredient FM composites with identical formulations were developed in the form of brake-pads. Out of which one composite series consisted of a single layer of Cu fabric in the body of brake-pad and designated as C1 while double layer of Cu fabric was incorporated in another brake-pad series with designation of C2. Distance of Cu fabric layer from the back-plate was kept constant for C1 and C2. One more composite (C0) was developed without Cu fabric for the sake of comparison. Developed composites were characterized for physical properties. Tribological performance was evaluated on full scale inertia dynamometer by following JASO C 406 testing standard. It was concluded that Cu fabric successfully improved fade resistance by increasing conductivity of the composite and also showed slight improvement in wear resistance. Worn surfaces of pads and disc were analyzed by SEM and EDAX to study wear mechanism.

Keywords: brake inertia dynamometer, copper fabric, non-asbestos organic (NAO) friction materials, thermal conductivity enhancement

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Authors: María Magdalena Méndez-González, Miguel García Rocha, Carlos Manuel Yermo De la Cruz

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Calcium phosphate (Ca5(PO4)3(X)) is widely used in orthopedic applications and is widely used as powder and granules. However, their presence in bone is in the form of nanometric needles 60 nm in length with a non-stoichiometric phase of apatite contains CO3-2, Na+, OH-, F-, and other ions in a matrix of collagen fibers. The crystal size, morphology control and interaction with cells are essential for the development of nanotechnology. The structural results of calcium phosphate, synthesized by chemical precipitation with crystal size of 22.85 nm are presented in this paper. The calcium phosphate powders were analyzed by X-ray diffraction, energy dispersive spectroscopy (EDS), infrared spectroscopy and FT-IR transmission electron microscopy. Network parameters, atomic positions, the indexing of the planes and the calculation of FWHM (full width at half maximum) were obtained. The crystal size was also calculated using the Scherer equation d (hkl) = cλ/βcosѲ. Where c is a constant related to the shape of the crystal, the wavelength of the radiation used for a copper anode is 1.54060Å, Ѳ is the Bragg diffraction angle, and β is the width average peak height of greater intensity. Diffraction pattern corresponding to the calcium phosphate called hydroxyapatite phase of a hexagonal crystal system was obtained. It belongs to the space group P63m with lattice parameters a = 9.4394 Å and c = 6.8861 Å. The most intense peak is obtained 2Ѳ = 31.55 (FWHM = 0.4798), with a preferred orientation in 121. The intensity difference between the experimental data and the calculated values is attributable to the temperature at which the sintering was performed. The intensity of the highest peak is at angle 2Ѳ = 32.11. The structure of calcium phosphate obtained was a hexagonal configuration. The intensity changes in the peaks of the diffraction pattern, in the lattice parameters at the corners, indicating the possible presence of a dopant. That each calcium atom is surrounded by a tetrahedron of oxygen and hydrogen was observed by infrared spectra. The unit cell pattern corresponds to hydroxyapatite and transmission electron microscopic crystal morphology corresponding to the hexagonal phase with a preferential growth along the c-plane was obtained.

Keywords: structure, nanoparticles, calcium phosphate, metallurgical and materials engineering

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Authors: Z. Mazrouei-Sebdani, A. Khoddami, H. Hadadzadeh, M. Zarrebini

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Silica aerogels are well-known meso-porous materials with high specific surface area (500–1000 m2/g), high porosity (80–99.8%), and low density (0.003–0.8 g/cm3). However, the silica aerogels generally are highly brittle due to their nanoporous nature. Physical and mechanical properties of the silica aerogels can be enhanced by compounding with the fibers. Although some reports presented incorporation of the fibers into the sol, followed by further modification and drying stages, no information regarding the aerogel powders as filler in the polymeric fibers is available. In this research, waterglass based aerogel powder was prepared in the following steps: sol–gel process to prepare a gel, followed by subsequent washing with propan-2-ol, n-Hexane, and TMCS, then ambient pressure drying, and ball milling. Inspired by limited dust releasing, aerogel powder was introduced to the PET electrospinning solution in an attempt to create required bulk and surface structure for the nano fibers to improve their hydrophobic and insulation properties. The samples evaluation was carried out by measuring density, porosity, contact angle, sliding angle, heat transfer, FTIR, BET and SEM. According to the results, porous silica aerogel powder was fabricated with mean pore diameter of 24 nm and contact angle of 145.9º. The results indicated the usefulness of the aerogel powder confined into nano fibers to control surface roughness for manipulating superhydrophobic nanowebs with sliding angle of 5˚ and water contact angle of 147º. It can be due to a multi-scale surface roughness which was created by nanowebs structure itself and nano fibers surface irregularity in presence of the aerogels while a laye of fluorocarbon created low surface energy. The wettability of a solid substrate is an important property that is controlled by both the chemical composition and geometry of the surface. Also, a decreasing trend in the heat transfer was observed from 22% for the nano fibers without any aerogel powder to 8% for the nano fibers with 4% aerogel powder. The development of thermal insulating materials has become increasingly more important than ever in view of the fossil energy depletion and global warming that call for more demanding energy-saving practices.

Keywords: Superhydrophobicity, Insulation, Sol-gel, Surface energy, Roughness.

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Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

Abstract:

The process of assembling metal nanoparticles at the interface of two liquids has received a great deal of attention over the past few years due to a wide range of important applications and their unusual properties as compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: Firstly, to describe the achievement of a closed loop recycling for producing cadmium sulfide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulfides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferrofluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Coinage metals like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: metal nanoparticles, core/shell structures and semiconductors, ferromagnetic properties, closed loop recycling, liquid/liquid interface

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Authors: Gonzalo Reyes, Magdalena Walczak, Esteban Ramos-Moore, Jorge Ramos-Grez

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Metal additive manufacture technologies have gained strong support and acceptance as a promising and alternative method to manufacture high performance complex geometry products. The main purpose of the present work is to study the microstructure and phase transformation temperatures of Cu-Al-Ni shape memory alloys fabricated from a direct laser additive process using metallic powders as precursors. The potential application is to manufacture self-centering seismic dampers for earthquake protection of buildings out of a copper based alloy by an additive process. In this process, the Cu-Al-Ni alloy is melted, inside of a high temperature and vacuum chamber with the aid of a high power fiber laser under inert atmosphere. The laser provides the energy to melt the alloy powder layer. The process allows fabricating fully dense, oxygen-free Cu-Al-Ni specimens using different laser power levels, laser powder interaction times, furnace ambient temperatures, and cooling rates as well as modifying concentration of the alloying elements. Two sets of specimens were fabricated with a nominal composition of Cu-13Al-3Ni and Cu-13Al-4Ni in wt.%, however, semi-quantitative chemical analysis using EDX examination showed that the specimens’ resulting composition was closer to Cu-12Al-5Ni and Cu-11Al-8Ni, respectively. In spite of that fact, it is expected that the specimens should still possess shape memory behavior. To confirm this hypothesis, phase transformation temperatures will be measured using DSC technique, to look for martensitic and austenitic phase transformations at 150°C. So far, metallographic analysis of the specimens showed defined martensitic microstructures. Moreover, XRD technique revealed diffraction peaks corresponding to (0 0 18) and (1 2 8) planes, which are too associated with the presence of martensitic phase. We conclude that it would be possible to obtain fully dense Cu-Al-Ni alloys having shape memory effect behavior by direct laser fabrication process, and to advance into fabrication of self centering seismic dampers by a controllable metal additive manufacturing process.

Keywords: Cu-Al-Ni alloys, direct laser fabrication, shape memory alloy, self-centering seismic dampers

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Authors: C. G. Mendez-Garcia, E. T. Romero-Guzman, H. Hernandez-Mendoza, C. Solis, E. Chavez-Lomeli, E. Chamizo, R. Garcia-Tenorio

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Plutonium is present in different concentrations in the environment and biological samples related to nuclear weapons testing, nuclear waste recycling and accidental discharges of nuclear plants. This radioisotope is considered the most radiotoxic substance, particularly when it enters the human body through inhalation of powders insoluble or aerosols. This is the main reason of the determination of the concentration of this radioisotope in the atmosphere. Besides that, the isotopic ratio of ²⁴⁰Pu/²³⁹Pu provides information about the origin of the source. PM₂.₅ sampling was carried out in the Metropolitan Zone of the Valley of Mexico (MZVM) from February 18th to March 17th in 2015 on quartz filter. There have been significant developments recently due to the establishment of new methods for sample preparation and accurate measurement to detect ultra trace levels as the plutonium is found in the environment. The accelerator mass spectrometry (AMS) is a technique that allows measuring levels of detection around of femtograms (10-15 g). The AMS determinations include the chemical isolation of Pu. The Pu separation involved an acidic digestion and a radiochemical purification using an anion exchange resin. Finally, the source is prepared, when Pu is pressed in the corresponding cathodes. According to the author's knowledge on these aerosols showed variations on the ²³⁵U/²³⁸U ratio of the natural value, suggesting that could be an anthropogenic source altering it. The determination of the concentration of the isotopes of Pu can be a useful tool in order the clarify this presence in the atmosphere. The first results showed a mean value of activity concentration of ²³⁹Pu of 280 nBq m⁻³ thus the ²⁴⁰Pu/²³⁹Pu was 0.025 corresponding to the weapon production source; these results corroborate that there is an anthropogenic influence that is increasing the concentration of radioactive material in PM₂.₅. According to the author's knowledge in Total Suspended Particles (TSP) have been reported activity concentrations of ²³⁹⁺²⁴⁰Pu around few tens of nBq m⁻³ and 0.17 of ²⁴⁰Pu/²³⁹Pu ratios. The preliminary results in MZVM show high activity concentrations of isotopes of Pu (40 and 700 nBq m⁻³) and low ²⁴⁰Pu/²³⁹Pu ratio than reported. These results are in the order of the activity concentrations of Pu in weapons-grade of high purity.

Keywords: aerosols, fallout, mass spectrometry, radiochemistry, tracer, ²⁴⁰Pu/²³⁹Pu ratio

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Authors: M. S. Abd El-Sadek, M. A. Omar, Gharib M. Taha

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In recent years, photocatalytic degradation of various kinds of organic and inorganic pollutants using semiconductor powders as photocatalysts has been extensively studied. Owing to its relatively high photocatalytic activity, biological and chemical stability, low cost, nonpoisonous and long stable life, Tin oxide materials have been widely used as catalysts in chemical reactions, including synthesis of vinyl ketone, oxidation of methanol and so on. Tin oxide (SnO₂), with a rutile-type crystalline structure, is an n-type wide band gap (3.6 eV) semiconductor that presents a proper combination of chemical, electronic and optical properties that make it advantageous in several applications. In the present work, SnO₂ nanoparticles were synthesized at room temperature by the sol-gel process and thermohydrolysis of SnCl₂ in isopropanol by controlling the crystallite size through calculations. The synthesized nanoparticles were identified by using XRD analysis, TEM, FT-IR, and Uv-Visible spectroscopic techniques. The crystalline structure and grain size of the synthesized samples were analyzed by X-Ray diffraction analysis (XRD) and the XRD patterns confirmed the presence of tetragonal phase SnO₂. In this study, Methylene blue degradation was tested by using SnO₂ nanoparticles (at different calculations temperatures) as a photocatalyst under sunlight as a source of irradiation. The results showed that the highest percentage of degradation of Methylene blue dye was obtained by using SnO₂ photocatalyst at calculations temperature 800 ᵒC. The operational parameters were investigated to be optimized to the best conditions which result in complete removal of organic pollutants from aqueous solution. It was found that the degradation of dyes depends on several parameters such as irradiation time, initial dye concentration, the dose of the catalyst and the presence of metals such as silver as a dopant and its concentration. Percent degradation was increased with irradiation time. The degradation efficiency decreased as the initial concentration of the dye increased. The degradation efficiency increased as the dose of the catalyst increased to a certain level and by further increasing the SnO₂ photocatalyst dose, the degradation efficiency is decreased. The best degradation efficiency on which obtained from pure SnO₂ compared with SnO₂ which doped by different percentage of Ag.

Keywords: SnO₂ nanoparticles, a sol-gel method, photocatalytic applications, methylene blue, degradation efficiency

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Authors: Elżbieta Cygan, Bączek, Piotr Wyżga

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This paper presents the results of research on the physical, mechanical, and tribological properties of materials constituting the matrix in sintered metallic-diamond tools. The ground powders based on the Fe-Mn-Cu-Sn-C system were modified with micro-sized particles of the ceramic phase: SiC, Al₂O₃ and consolidated using the SPS (spark plasma sintering) method to a relative density of over 98% at 850-950°C, at a pressure of 35 MPa and time 10 min. After sintering, an analysis of the microstructure was conducted using scanning electron microscopy. The resulting materials were tested for the apparent density determined by Archimedes’ method, Rockwell hardness (scale B), Young’s modulus, as well as for technological properties. The performance results of obtained diamond composites were compared with the base material (Fe–Mn–Cu–Sn–C) and the commercial alloy Co-20% WC. The hardness of composites has achieved the maximum at a temperature of 900°C; therefore, it should be considered that at this temperature it was obtained optimal physical and mechanical properties of the subjects' composites were. Research on tribological properties showed that the composites modified with micro-sized particles of the ceramic phase are characterized by more than twice higher wear resistance in comparison with base materials and the commercial alloy Co-20% WC. Composites containing Al₂O₃ phase particles in the matrix material were composites containing Al₂O₃ phase particles in the matrix material were characterized by the lowest abrasion wear resistance. The manufacturing technology presented in the paper is economically justified and can be successfully used in the production process of the matrix in sintered diamond-impregnated tools used for the machining of an industrial floor system. Acknowledgment: The study was performed under LIDER IX Research Project No. LIDER/22/0085/L-9/17/NCBR/2018 entitled “Innovative metal-diamond tools without the addition of critical raw materials for applications in the process of grinding industrial floor systems” funded by the National Centre for Research and Development of Poland, Warsaw.

Keywords: abrasive wear resistance, metal matrix composites, sintered diamond tools, Spark Plasma Sintering

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Authors: Paulina Zavistanaviciute, Vita Krungleviciute, Elena Bartkiene

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Lactic acid bacteria (LAB) are microbial supplements that increase the nutritional, therapeutic, and safety value of food and feed. Often LAB strains are incubated in an expensive commercially available de Man-Rogosa-Sharpe (MRS) medium; the cultures are centrifuged, and the cells are washing with sterile water. Potato juice and apple juice industry bio-products are industrial wastes which may constitute a source of digestible nutrients for microorganisms. Due to their low cost and good chemical composition, potato juice and apple juice production bio- products could have a potential application in LAB encapsulation. In this study, pure LAB (P. acidilactici and P. pentosaceus) were multiplied in a crushed potato juice and apple juice industry bio-products medium. Before using, bio-products were sterilized and filtered. No additives were added to mass, except apple juice industry bioproducts were diluted with sterile water (1/5; v/v). The tap of sterilised mass, and LAB cell suspension (5 mL), containing of 8.9 log10 colony-forming units (cfu) per mL of the P. acidilactici and P. pentosaceus was used to multiply the LAB for 72 h. The final colony number in the potato juice and apple juice bio- products substrate was on average 9.60 log10 cfu/g. In order to stabilize the LAB, several methods of dehydration have been tested: lyophilisation (MilrockKieffer Lane, Kingston, USA) and dehydration in spray drying system (SD-06, Keison, Great Britain). Into the spray drying system multiplied LAB in a crushed potato juice and apple juice bio-products medium was injected in peristaltic way (inlet temperature +60 °C, inlet air temperature +150° C, outgoing air temperature +80 °C, air flow 200 m3/h). After lyophilisation (-48 °C) and spray drying (+150 °C) the viable cell concentration in the fermented potato juice powder was 9.18 ± 0.09 log10 cfu/g and 9.04 ± 0.07 log10 cfu/g, respectively, and in apple mass powder 8.03 ± 0.04 log10 cfu/g and 7.03 ± 0.03 log10 cfu/g, respectively. Results indicated that during the storage (after 12 months) at room temperature (22 +/- 2 ºC) LAB count in dehydrated products was 5.18 log10 cfu/g and 7.00 log10 cfu/g (in spray dried and lyophilized potato juice powder, respectively), and 3.05 log10 cfu/g and 4.10 log10 cfu/g (in spray dried and lyophilized apple juice industry bio-products powder, respectively). According to obtained results, potato juice could be used as alternative substrate for P. acidilactici and P. pentosaceus cultivation, and by drying received powders can be used in food/feed industry as the LAB starters. Therefore, apple juice industry by- products before spray drying and lyophilisation should be modified (i. e. by using different starches) in order to improve its encapsulation.

Keywords: bio-products, encapsulation, lactic acid bacteria, sustainability

Procedia PDF Downloads 253

Authors: Shian Guan, Marie Bourdin, Isabelle Trenque, Younes Messaddeq, Thierry Cardinal, Nicolas Penin, Issam Mjejri, Aline Rougier, Etienne Duguet, Stephane Mornet, Manuel Gaudon

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At the interface of the studies performed by 3 Ph.D. students: Shian Guan (2017-2020), Marie Bourdin (2016-2019) and Isabelle Trenque (2012-2015), a single synthesis route: polyol-mediated process, was used with success for the preparation of different inorganic oxides. Both of these inorganic oxides were elaborated for their potential application as smart optical compounds. This synthesis route has allowed us to develop nanoparticles of zinc oxide, vanadium oxide or tungsten oxide. This route is with easy implementation, inexpensive and with large-scale production potentialities and leads to materials of high purity. The obtaining by this route of nanometric particles, however perfectly crystalline, has notably led to the possibility of doping these matrix materials with high doping ion concentrations (high solubility limits). Thus, Al3+ or Ga3+ doped-ZnO powder, with high doping rate in comparison with the literature, exhibits remarkable infrared absorption properties thanks to their high free carrier density. Note also that due to the narrow particle size distribution of the as-prepared nanometric doped-ZnO powder, the original correlation between crystallite size and unit-cell parameters have been established. Also, depending on the annealing atmosphere use to treat vanadium precursors, VO2, V2O3 or V2O5 oxides with thermochromic or electrochromic properties can be obtained without any impurity, despite the versatility of the oxidation state of vanadium. This is of more particular interest on vanadium dioxide, a relatively difficult-to-prepare oxide, whose first-order metal-insulator phase transition is widely explored in the literature for its thermochromic behavior (in smart windows with optimal thermal insulation). Finally, the reducing nature of the polyol solvents ensures the production of oxygen-deficient tungsten oxide, thus conferring to the nano-powders exotic colorimetric properties, as well as optimized photochromic and electrochromic behaviors.

Keywords: inorganic oxides, electrochromic, photochromic, thermochromic

Procedia PDF Downloads 194

Authors: Y. Sakai, C. Wang

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The decrease in agricultural production due to soil deterioration has been an urgent task. Soil acidification is a potentially serious land degradation issue and it will have a major impact on agricultural productivity and sustainable farming systems. In China, acid soil is mainly distributed in the southern part, the decrease in agricultural production and heavy metal contamination are serious problems. In addition, not only environmental and health problems due to the exhaust gas such as mainly sulfur dioxide (SO₂) but also the generation of a huge amount of construction and demolition wastes with the accelerating urbanization has emerged as a social problem in China. Therefore, the need for the recycling and reuse of both desulfurization waste and waste concrete is very urgent and necessary. So we have investigated the effectiveness as acid soil amendments of both coal bio-briquette ash and waste concrete. In this paper, acid soil (AS1) in Nanjing (pH=6.0, EC=1.6dSm-1) and acid soil (AS2) in Guangzhou (pH=4.1, EC=0.2dSm-1) were investigated in soil amelioration test. Soil amendments were three coal bio-briquette ashes (BBA1, BBA2 and BBA3), the waste cement fine powders (CFP) ( < 200µm (particle diameter)), waste concrete particles (WCP) ( < 4.75mm ( < 0.6mm, 0.6-1.0mm, 1.0-2.0mm, 2.0-4.75mm)), and six mixtures with two coal bio-briquette ashes (BBA2 and BBA3), CFP, WCP( < 0.6mm) and WCP(2.0-4.75mm). In acid soil amelioration test, the three BBAs, CFP and various WCPs based on exchangeable calcium concentration were added to two acid soils. The application rates were from 0 wt% to 3.5 wt% in AS1 test and from 0 wt% to 6.0 wt% in AS2 test, respectively. Soil chemical properties (pH, EC, exchangeable and soluble ions (Na, Ca, Mg, K)) before and after mixing with soil amendments were measured. In addition, Al toxicity and the balance of salts (CaO, K₂O, MgO) in soil after amelioration was evaluated. The order of pH and exchangeable Ca concentration that is effective for acid soil amelioration was WCP(0.6mm) > CFP > WCP(2.0-4.25mm) > BB1 > BB2 > BB3. In all AS 1 and AS 2 amelioration tests using three BBAs, the pH and EC increased slightly with the increase of application rate and reached to the appropriate value range of both pH and EC in BBA1 only. Because BBA1 was higher value in pH and exchangeable Ca. After that, soil pH and EC with the increase in the application rate of BBA2, BBA3 and by using CFP, WC( < 0.6mm), WC(2.0-4.75mm) as soil amendment reached to each appropriate value range, respectively. In addition, the mixture amendments with BBA2, BBA3 CFP, WC( < 0.6mm), and WC(2.0-4.75mm) could ameliorate at a smaller amount of application rate in case of BBA only. And the exchangeable Al concentration decreased drastically with the increase in pH due to soil amelioration and was under the standard value. Lastly, the heavy metal (Cd, As, Se, Ni, Cr, Pb, Mo, B, Cu, Zn) contents in new soil amendments were under control standard values for agricultural use in China. Thus we could propose a new acid soil amelioration method using coal bio-briquette ash and waste concrete in China.

Keywords: acid soil, coal bio-briquette ash, soil amelioration, waste concrete

Procedia PDF Downloads 157

Authors: Aaron Herve Mbwe Mbissik, Lotfi Khiari, Otmane Raji, Abdellatif Elghali, Abdelkarim Lajili, Muhammad Ouabid, Martin Jemo, Jean-Louis Bodinier

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Potassium (K) is an essential macronutrient for plant growth, helping to regulate several physiological and metabolic processes. Evaporite-related potash salts, mainly sylvite minerals (K chloride or KCl), are the principal source of K for the fertilizer industry. However, due to the high potash-supply risk associated with its considerable price fluctuations and uneven geographic distribution for most agriculture-based developing countries, the development of alternative sources of fertilizer K is imperative to maintain adequate crop yield, reduce yield gaps, and food security. Alkaline Igneous rocks containing significant K-rich silicate minerals such as K feldspar are increasingly seen as the best alternative available. However, these rocks may require to be hydrothermally treatment to enhance the release of potassium. In this study, we evaluate the fertilizing capacity of raw and hydrothermally treated K-bearing silicate rocks from different areas in Morocco. The effectiveness of rock powders was tested in a greenhouse experiment using ryegrass (Lolium multiflorum) by comparing them to a control (no K added) and to a conventional fertilizer (muriate of potash: MOP or KCl). The trial was conducted in a randomized complete block design with three replications, and plants were grown on K-depleted soils for three growing cycles. To achieve our objective, in addition to the analysis of the muriate response curve and the different biomasses, we also examined three necessary coefficients, namely: the K uptake, then apparent K recovery (AKR), and the relative K efficiency (RKE). The results showed that based on the optimum economic rate of MOP (230 kg.K.ha⁻¹) and the optimum yield (44 000 kg.K.ha⁻¹), the efficiency of K silicate rocks was as high as that of MOP. Although the plants took up only half of the K supplied by the powdered rock, the hydrothermal material was found to be satisfactory, with a biomass value reaching the optimum economic limit until the second crop cycle. In comparison, the AKR of the MOP (98.6%) and its RKE in the 1st cycle were higher than our materials: 39% and 38%, respectively. Therefore, the raw and hydrothermal materials mixture could be an appropriate solution for long-term agronomic use based on the obtained results.

Keywords: K-uptake, AKR, RKE, K-bearing silicate rock, MOP

Procedia PDF Downloads 58

Authors: Irene Buj-Corral, Ali Bagheri, Alejandro Dominguez-Fernandez

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In recent years, use of ceramic prostheses as an implant in some parts of body has become common. In the present study, research has focused on replacement of the acetabulum bone, which is a part of the pelvis bone. Metallic prostheses have shown some problems such as release of metal ions into patient's blood. In addition, fracture of liners and squeezing between surface of femoral head and inner surface of acetabulum have been reported. Ceramic prostheses have the advantage of low debris and high strength, although they are more difficult to be manufactured than metallic ones. Specifically, new designs try to attempt an acetabulum in which the outer surface will be porous for proliferation of cells and fixation of the prostheses by means of osteointegration, while inner surface must be smooth enough to assure that the movement between femoral head and inner surface will be carried out with on feasibility. In the present study, 3D printing technologies are used for manufacturing ceramic prostheses. In Fused Deposition Modelling (FDM) process, 3D printed plastic prostheses are obtained by means of melting of a plastic filament and subsequent deposition on a glass surface. A similar process is applied to ceramics in which ceramic powders need to be mixed with a liquid polymer before depositing them. After 3D printing, parts are subjected to a sintering process in an oven so that they can achieve final strength. In the present paper, influence of printing parameters on surface roughness 3D printed ceramic parts are presented. Three parameter full factorial design of experiments was used. Selected variables were layer height, infill and nozzle diameter. Responses were average roughness Ra and mean roughness depth Rz. Regression analysis was applied to responses in order to obtain mathematical models for responses. Results showed that surface roughness depends mainly on layer height and nozzle diameter employed, while infill was found not to be significant. In order to get low surface roughness, low layer height and low infill should be selected. As a conclusion, layer height and infill are important parameters for obtaining good surface finish in ceramic 3D printed prostheses. However, use of too low infill could lead to prostheses with low mechanical strength. Such prostheses could not be able to bear the static and dynamic charges to which they are subjected once they are implanted in the body. This issue will be addressed in further research.

Keywords: ceramic, hip prostheses, surface roughness, 3D printing

Procedia PDF Downloads 166

Authors: Nur Azilina Abdul Aziz, Tuti Katrina Abdullah, Ahmad Azmin Mohamad

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Lithium-transition metals and some of their oxides, such as LiCoO2, LiMn2O2, LiFePO4, and LiNiO2 have been used as cathode materials in high performance lithium-ion rechargeable batteries. Among the cathode materials, LiCoO2 has potential to been widely used as a lithium-ion battery because of its layered crystalline structure, good capacity, high cell voltage, high specific energy density, high power rate, low self-discharge, and excellent cycle life. This cathode material has been widely used in commercial lithium-ion batteries due to its low irreversible capacity loss and good cycling performance. However, there are several problems that interfere with the production of material that has good electrochemical properties, including the crystallinity, the average particle size and particle size distribution. In recent years, synthesis of nanoparticles has been intensively investigated. Powders prepared by the traditional solid-state reaction have a large particle size and broad size distribution. On the other hand, solution method can reduce the particle size to nanometer range and control the particle size distribution. In this study, LiCoO2 was synthesized using the sol–gel preparation method, which Lithium acetate and Cobalt acetate were used as reactants. The stoichiometric amounts of the reactants were dissolved in deionized water. The solutions were stirred for 30 hours using magnetic stirrer, followed by heating at 80°C under vigorous stirring until a viscous gel was formed. The as-formed gel was calcined at 700°C for 7 h under a room atmosphere. The structural and morphological analysis of LiCoO2 was characterized using X-ray diffraction and Scanning electron microscopy. The diffraction pattern of material can be indexed based on the α-NaFeO2 structure. The clear splitting of the hexagonal doublet of (006)/(102) and (108)/(110) in this patterns indicates materials are formed in a well-ordered hexagonal structure. No impurity phase can be seen in this range probably due to the homogeneous mixing of the cations in the precursor. Furthermore, SEM micrograph of the LiCoO2 shows the particle size distribution is almost uniform while particle size is between 0.3-0.5 microns. In conclusion, LiCoO2 powder was successfully synthesized using the sol–gel method. LiCoO2 showed a hexagonal crystal structure. The sample has been prepared clearly indicate the pure phase of LiCoO2. Meanwhile, the morphology of the sample showed that the particle size and size distribution of particles is almost uniform.

Keywords: cathode material, LiCoO2, lithium-ion rechargeable batteries, Sol-Gel method

Procedia PDF Downloads 331

Authors: Vladimir Hovhannisyan, Chen Yuan Dong

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Recently nanoparticles (NPs) have been introduced in biomedicine as effective agents for cancer-targeted drug delivery and noninvasive tissue imaging. The most important requirements to these agents are their non-toxicity, biocompatibility and stability. In view of these criteria, the zeolite (ZL) nanoparticles (NPs) may be considered as perfect candidates for biomedical applications. ZLs are crystalline aluminosilicates consisting of oxygen-sharing SiO4 and AlO4 tetrahedral groups united by common vertices in three-dimensional framework and containing pores with diameters from 0.3 to 1.2 nm. Generally, the behavior and physical properties of ZLs are studied by SEM, X-ray spectroscopy, and AFM, whereas optical spectroscopic and microscopic approaches are not effective enough, because of strong scattering in common ZL bulk materials and powders. The light scattering can be reduced by using of ZL NPs. ZL NPs have large external surface area, high dispersibility in both aqueous and organic solutions, high photo- and thermal stability, and exceptional ability to adsorb various molecules and atoms in their nanopores. In this report, using multiphoton microscopy and nonlinear spectroscopy, we investigate nonlinear optical properties of clinoptilolite type of ZL micro- and nanoparticles with average diameters of 2200 nm and 240 nm, correspondingly. Multiphoton imaging is achieved using a laser scanning microscope system (LSM 510 META, Zeiss, Germany) coupled to a femtosecond titanium:sapphire laser (repetition rate- 80 MHz, pulse duration-120 fs, radiation wavelength- 720-820 nm) (Tsunami, Spectra-Physics, CA). Two Zeiss, Plan-Neofluar objectives (air immersion 20×∕NA 0.5 and water immersion 40×∕NA 1.2) are used for imaging. For the detection of the nonlinear response, we use two detection channels with 380-400 nm and 435-700 nm spectral bandwidths. We demonstrate that ZL micro- and nanoparticles can produce nonlinear optical response under the near-infrared femtosecond laser excitation. The interaction of hypericine, chlorin e6 and other dyes with ZL NPs and their photodynamic activity is investigated. Particularly, multiphoton imaging shows that individual ZL NPs particles adsorb Zn-tetraporphyrin molecules, but do not adsorb fluorescein molecules. In addition, nonlinear spectral properties of ZL NPs in native biotissues are studied. Nonlinear microscopy and spectroscopy may open new perspectives in the research and application of ZL NP in biomedicine, and the results may help to introduce novel approaches into the clinical environment.

Keywords: multiphoton microscopy, nanoparticles, nonlinear optics, zeolite

Procedia PDF Downloads 391

Authors: Jin Li, Jing Sun, Xiangkun Cai, Lijuanwang, Yanbin Tang, Junsheng Huo

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In order to improve the malnutrition of infants and young children in poor rural areas of China, Chinese government implement a project on improvement of children's nutrition in poor rural areas. Each infant or young child aged 6 to 23 months in selected poor rural areas of China was provided a package of Yingyangbao (YYB) per day, which is a full fat soy powder mixed with multiple micronutrient powders. A technical direction to implement this project comprehensively in poor rural areas of China will be provided by assessing the nutritional status of infants and feeding practices of caregiver. The nutritional intervention was conducted using Yingyangbao for infants aged 6 to 23 months in six poor counties of Shanxi, Yunnan and Hubei Provinces. The caregiver or parents of infants were educated on feeding knowledge and practice. A total of 1840 infants were assessed before the intervention and 1789 infants one year later. The length, weight, hemoglobin concentration of infants were measured to evaluate nutritional status before and after the intervention respectively. The questionnaires were designed to collect data for the basic demographic information and feeding practices. The average weight of infants aged 6 to 23 months increased from 9.59 ± 1.54kg to 9.73 ± 1.61kg one years later (p<0.01), and the average length from 76.0±6.0 to 77.0±6.1(p<0.01). The weight and length of infants aged 12 to 17 months had most obviously improving effect among the three age groups. Before the intervention, the hemoglobin concentration value of infants was 11.7±1.2g/L, and the anemia prevalence was 32.9%. One year later, the hemoglobin concentration value of the infants was increased to 12.0±1.1g/dL, and the anemia prevalence was decreased to 26.0%. There were both statistically significant (p <0.01). The anemia prevalence of infants aged 18 to 23 months had most obviously improving effect，which decreased from 25.0% to 17.2%(p<0.01). The proportion of infants aged 6 to 8 months who received solid, semi-solid or soft foods in time was increased from 89.4% to 91.6%, while there was no statistically significant. The proportion of 6-23 month-old infants who received minimum dietary diversity increased from 55.6% to 60.3%(p <0.01). The differences of the proportion of infants who received minimum meal frequency was no statistically significant between before and after the intervention. The nutritional intervention using Yingyangbao showed the significant effect for improving infants aged 6 to 23 months anemia status, weight and length. The feeding practices were improved through education in the process of nutritional intervention, while the effect is not significant. It is need for Chinese government to explore new publicity pattern.

Keywords: nutritional intervention, infants, nutritional status, feeding practice

Procedia PDF Downloads 415

Authors: A. S. V. Carvalho, J. Luis, L. S. O. Pires, J. M. Oliveira

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Additive manufacturing technologies (AM) experienced a remarkable growth in the latest years due to the development and diffusion of a wide range of three-dimensional (3D) printing techniques. Nowadays we can find techniques available for non-industrial users, like fused filament fabrication, but techniques like 3D printing, polyjet, selective laser sintering and stereolithography are mainly spread in the industry. Robocasting (R3D) shows a great potential due to its ability to shape materials with a wide range of viscosity. Industrial porcelain compositions showing different rheological behaviour can be prepared and used as candidate materials to be processed by R3D. The use of this AM technique in industry is very residual. In this work, a specific porcelain composition with suitable rheological properties will be processed by R3D, and a systematic study of the printing parameters tuning will be shown. The porcelain composition was formulated based on an industrial spray dried porcelain powder. The powder particle size and morphology was analysed. The powders were mixed with water and an organic binder on a ball mill at 200 rpm/min for 24 hours. The batch viscosity was adjusted by the addition of an acid solution and mixed again. The paste density, viscosity, zeta potential, particle size distribution and pH were determined. In a R3D system, different speed and pressure settings were studied to access their impact on the fabrication of porcelain models. These models were dried at 80 °C, during 24 hours and sintered in air at 1350 °C for 2 hours. The stability of the models, its walls and surface quality were studied and their physical properties were accessed. The microstructure and layer adhesion were observed by SEM. The studied processing parameters have a high impact on the models quality. Moreover, they have a high impact on the stacking of the filaments. The adequate tuning of the parameters has a huge influence on the final properties of the porcelain models. This work contributes to a better assimilation of AM technologies in ceramic industry. Acknowledgments: The RoboCer3D project – project of additive rapid manufacturing through 3D printing ceramic material (POCI-01-0247-FEDER-003350) financed by Compete 2020, PT 2020, European Regional Development Fund – FEDER through the International and Competitive Operational Program (POCI) under the PT2020 partnership agreement.

Keywords: additive manufacturing, porcelain, robocasting, R3D

Procedia PDF Downloads 138

Authors: Elvan G. Bulut, Betul Goksun, Tugba G. Gun, Ozge Sakiyan Demirkol, Kamuran Ayhan, Kezban Candogan

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Dysphagia, difficulty in swallowing solid foods and thin liquids, is one of the common health threats among the elderly who require foods with modified texture in their diet. Although there are some commercial food formulations or hydrocolloids to thicken the liquid foods for dysphagic individuals, there is still a need for developing and offering new food products with enriched nutritional, textural and sensory characteristics to safely nourish these patients. 3D food printing is an appealing alternative in creating personalized foods for this purpose with attractive shape, soft and homogenous texture. In order to modify texture and prevent phase separation, hydrocolloids are generally used. In our laboratory, an optimized 3D printed beef-based formulation specifically for people with swallowing difficulties was developed based on the research project supported by the Scientific and Technological Research Council of Turkey (TÜBİTAK Project # 218O017). The optimized formulation obtained from response surface methodology was 60% beef powder, 5.88% gelatin, and 0.74% kappa-carrageenan (all in a dry basis). This product was enriched with powders of freeze-dried beet, celery, and red capia pepper, butter, and whole milk. Proximate composition (moisture, fat, protein, and ash contents), pH value, CIE lightness (L*), redness (a*) and yellowness (b*), and color difference (ΔE*) values were determined. Counts of total mesophilic aerobic bacteria (TMAB), lactic acid bacteria (LAB), mold and yeast, total coliforms were conducted, and detection of coagulase positive S. aureus, E. coli, and Salmonella spp. were performed. The 3D printed products had 60.11% moisture, 16.51% fat, 13.68% protein, and 1.65% ash, and the pH value was 6.19, whereas the ΔE* value was 3.04. Counts of TMAB, LAB, mold and yeast and total coliforms before and after 3D printing were 5.23-5.41 log cfu/g, < 1 log cfu/g, < 1 log cfu/g, 2.39-2.15 log EMS/g, respectively. Coagulase positive S. aureus, E. coli, and Salmonella spp. were not detected in the products. The data obtained from this study based on determining some important product characteristics of functional beef-based formulation provides an encouraging basis for future research on the subject and should be useful in designing mass production of 3D printed products of similar composition.

Keywords: beef, dysphagia, product characteristics, texture-modified foods, 3D food printing

Procedia PDF Downloads 85

Authors: Julia Cristina Bonaldo, Christophe L. Martin, Severine Romero Baivier, Stephane Mazerat

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Alumina refractories are commonly used in steel and foundry industries. These refractories are prepared through a powder metallurgy route. They are a mixture of hard alumina particles and graphite platelets embedded into a soft carbonic matrix (binder). The powder can be cold pressed isostatically or uniaxially, depending on the application. The compact is then fired to obtain the final product. The quality of the product is governed by the microstructure of the composite and by the process parameters. The compaction behavior and the mechanical properties of the fired product depend greatly on the amount of each phase, on their morphology and on the initial microstructure. In order to better understand the link between these parameters and the macroscopic behavior, we use the Discrete Element Method (DEM) to simulate the compaction process and the fracture behavior of the fired composite. These simulations are coupled with well-designed experiments. Four mixes with various amounts of Al₂O₃ and binder were tested both experimentally and numerically. In DEM, each particle is modelled and the interactions between particles are taken into account through appropriate contact or bonding laws. Here, we model a bimodal mixture of large Al₂O₃ and small Al₂O₃ covered with a soft binder. This composite is itself mixed with graphite platelets. X-ray tomography images are used to analyze the morphologies of the different components. Large Al₂O₃ particles and graphite platelets are modelled in DEM as sets of particles bonded together. The binder is modelled as a soft shell that covers both large and small Al₂O₃ particles. When two particles with binder indent each other, they first interact through this soft shell. Once a critical indentation is reached (towards the end of compaction), hard Al₂O₃ - Al₂O₃ contacts appear. In accordance with experimental data, DEM simulations show that the amount of Al₂O₃ and the amount of binder play a major role for the compaction behavior. The graphite platelets bend and break during the compaction, also contributing to the macroscopic stress. Firing step is modeled in DEM by ascribing bonds to particles which contact each other after compaction. The fracture behavior of the compacted mixture is also simulated and compared with experimental data. Both diametrical tests (Brazilian tests) and triaxial tests are carried out. Again, the link between the amount of Al₂O₃ particles and the fracture behavior is investigated. The methodology described here can be generalized to other particulate materials that are used in the ceramic industry.

Keywords: cold compaction, composites, discrete element method, refractory materials, x-ray tomography

Procedia PDF Downloads 114

Authors: Emmanuel Ikechuckwu Onwubuya, Afees Adebayo Oladejo

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Background: The use of medicinal plants in the treatment of chronic diseases especially myocardial infarction, is gaining wide acceptance globally. Andrographis paniculata (Acanthaceae) is a medicinal plant commonly known as the king of bitters in Nigeria and has been acclaimed for several therapeutic activities. Materials and methods: This study investigated the cardio-protective effect of the leaf extract of A. paniculata in isoproterenol-induced myocardial infarction. Fresh green leaves of A paniculata were harvested from the Faculty of Agriculture farmland, Nnamdi Azikiwe University, Awka, Nigeria. Identification and authentication of the plant were carried out at the Department of Botany, Nnamdi Azikiwe University and a voucher specimen was deposited at the herbarium. The plant material was then shredded, air-dried under shade and pulverized. The fine powders obtained were weighed and extraction was done via a solvent combination of water and ethanol (3:7) for 72 hr via maceration. The filtrate gotten was evaporated to dryness to obtain the ethanol extract, which was used for further bioassay study. The bioactive constituents of the plant extract were quantitatively analyzed by Gas chromatography-mass spectrometry (GC-MS). The animals were administered the extract of A. paniculata orally for seven days at a divided dose of 100 mg/kg, 200 mg/kg and 400 mg/kg body weights. On the eighth day, myocardial infarction was induced through subcutaneous administration of isoproterenol at a dose of 150 mg/kg/day diluted in 2 ml of saline on two consecutive days. Subsequently, the blood pressures were monitored and blood was collected for bioassay studies. Results: The results of the study showed that the leaf extract of A. paniculata was rich in Dodecanoic acid (8.261%), 4-Dibenzofuranamine (6.03%), Cyclotrisiloxane (4.679 %). The findings also showed a significant decrease (p>0.05) in the Mean arterial blood pressure, heart rate, aspartate transaminase, alanine transaminase, creatinine kinase and lactate dehydrogenase activities of the treatment group compared with the untreated control group while the antioxidant (superoxide dismutase, catalase and glutathione) activities were significantly increased in the treatment group, compared with the untreated control group. Conclusion: The findings of this work have shown that the leaf of A. paniculata was rich in bioactive compounds, which could be synthesized to produce plant-based products to fight cardiovascular diseases, especially myocardial infarction.

Keywords: cardiovascular disease, myocardial infarction, medicinal plant, andrographis paniculata, isoproterenol

Procedia PDF Downloads 83

Authors: Jing-Yang Chung, Chi-Wei Liao, Jing Li, Bor Kae Chang, Cheng-Yu Wang

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Chemical hydride ammonia borane (AB, NH3BH3) draws attentions to hydrogen energy researches for its high theoretical gravimetrical capacity (19.6 wt%). Nevertheless, the elevated AB decomposition temperatures (Td) and unwanted byproducts are main hurdles in practical application. It was reported that the byproducts and Td can be reduced with nanoconfinement technique, in which AB molecules are confined in porous materials, such as porous carbon, zeolite, metal-organic frameworks (MOFs), etc. Although nanoconfinement empirically shows effectiveness on hydrogen generation temperature reduction in AB, the theoretical mechanism is debatable. Low Td was reported in AB@IRMOF-1 (Zn4O(BDC)3, BDC = benzenedicarboxylate), where Zn atoms form closed metal clusters secondary building unit (SBU) with no exposed active sites. Other than nanosized hydride, it was also observed that catalyst addition facilitates AB decomposition in the composite of Li-catalyzed carbon CMK-3, MOF JUC-32-Y with exposed Y3+, etc. It is believed that nanosized AB is critical for lowering Td, while active sites eliminate byproducts. Nonetheless, some researchers claimed that it is the catalytic sites that are the critical factor to reduce Td, instead of the hydride size. The group physically ground AB with ZIF-8 (zeolitic imidazolate frameworks, (Zn(2-methylimidazolate)2)), and found similar reduced Td phenomenon, even though AB molecules were not ‘confined’ or forming nanoparticles by physical hand grinding. It shows the catalytic reaction, not nanoconfinement, leads to AB dehydrogenation promotion. In this research, we explored the possible criteria of hydrogen production temperature from nanoconfined AB in MOFs with different pore sizes and active sites. MOFs with metal SBU such as Zn (IRMOF), Zr (UiO), and Al (MIL-53), accompanying with various organic ligands (BDC and BPDC; BPDC = biphenyldicarboxylate) were modified with AB. Excess MOFs were used for AB size constrained in micropores estimated by revisiting Horvath-Kawazoe model. AB dissolved in methanol was added to MOFs crystalline with MOF pore volume to AB ratio 4:1, and the slurry was dried under vacuum to collect AB@MOF powders. With TPD-MS (temperature programmed desorption with mass spectroscopy), we observed Td was reduced with smaller MOF pores. For example, it was reduced from 100°C to 64°C when MOF micropore ~1 nm, while ~90°C with pore size up to 5 nm. The behavior of Td as a function of AB crystalline radius obeys thermodynamics when the Gibbs free energy of AB decomposition is zero, and no obvious correlation with metal type was observed. In conclusion, we discovered Td of AB is proportional to the reciprocal of MOF pore size, possibly stronger than the effect of active sites.

Keywords: ammonia borane, chemical hydride, metal-organic framework, nanoconfinement

Procedia PDF Downloads 157

Authors: T. Kuchukhidze, N. Jalagonia, T. Archuadze, G. Bokuchava

Abstract:

The growing scientific-technological progress in modern civilization causes actuality of producing construction materials which can successfully work in conditions of high temperature, radiation, pressure, speed, and chemically aggressive environment. Such extreme conditions can withstand very few types of materials and among them, ceramic materials are in the first place. Corundum ceramics is the most useful material for creation of constructive nodes and products of various purposes for its low cost, easy accessibility to raw materials and good combination of physical-chemical properties. However, ceramic composite materials have one disadvantage; they are less plastics and have lower toughness. In order to increase the plasticity, the ceramics are reinforced by various dopants, that reduces the growth of the cracks. It is shown, that adding of even small amount of carbon fibers and carbon nanotubes (CNT) as reinforcing material significantly improves mechanical properties of the products, keeping at the same time advantages of alundum ceramics. Graphene in composite material acts in the same way as inorganic dopants (MgO, ZrO2, SiC and others) and performs the role of aluminum oxide inhibitor, as it creates shell, that gives possibility to reduce sintering temperature and at the same time it acts as damper, because scattering of a shock wave takes place on carbon structures. Application of different structural modification of carbon (graphene, nanotube and others) as reinforced material, gives possibility to create multi-purpose highly requested composite materials based on alundum ceramics. In the present work offers simplified technology for obtaining of aluminum oxide ceramics, reinforced with carbon nanostructures, during which chemical modification with doping carbon nanostructures will be implemented in the process of synthesis of final powdery composite – Alumina. In charge doping carbon nanostructures connected to matrix substance with C-O-Al bonds, that provide their homogeneous spatial distribution. In ceramic obtained as a result of consolidation of such powders carbon fragments equally distributed in the entire matrix of aluminum oxide, that cause increase of bending strength and crack-resistance. The proposed way to prepare the charge simplifies the technological process, decreases energy consumption, synthesis duration and therefore requires less financial expenses. In the implementation of this work, modern instrumental methods were used: electronic and optical microscopy, X-ray structural and granulometric analysis, UV, IR, and Raman spectroscopy.

Keywords: ceramic materials, α-Al₂O₃, carbon nanostructures, composites, characterization, hot-pressing

Procedia PDF Downloads 92

Authors: Josef Drahorad, Milos Beran, Ondrej Vltavsky, Marian Urban, Martin Fronek, Jiri Sova

Abstract:

Engineering efforts of researchers of the Food research institute Prague and the Czech Technical University in spray drying technologies led to the introduction of a demonstrator ATOMIZER and a new technology of Carbon Dioxide-Assisted Spray Nebulization Drying (CASND). The equipment combines the spray drying technology, when the liquid to be dried is atomized by a rotary atomizer, with Carbon Dioxide Assisted Nebulization - Bubble Dryer (CAN-BD) process in an original way. A solution, emulsion or suspension is saturated by carbon dioxide at pressure up to 80 bar before the drying process. The atomization process takes place in two steps. In the first step, primary droplets are produced at the outlet of the rotary atomizer of special construction. In the second step, the primary droplets are divided in secondary droplets by the CO2 expansion from the inside of primary droplets. The secondary droplets, usually in the form of microbubbles, are rapidly dried by warm air stream at temperatures up to 60ºC and solid particles are formed in a drying chamber. Powder particles are separated from the drying air stream in a high efficiency fine powder separator. The product is frequently in the form of submicron hollow spheres. The CASND technology has been used to produce microparticulated protein concentrates for human nutrition from alternative plant sources - hemp and canola seed filtration cakes. Alkali extraction was used to extract the proteins from the filtration cakes. The protein solutions after the alkali extractions were dried with the demonstrator ATOMIZER. Aerosol particle size distribution and concentration in the draying chamber were determined by two different on-line aerosol spectrometers SMPS (Scanning Mobility Particle Sizer) and APS (Aerodynamic Particle Sizer). The protein powders were in form of hollow spheres with average particle diameter about 600 nm. The particles were characterized by the SEM method. The functional properties of the microparticulated protein concentrates were compared with the same protein concentrates dried by the conventional spray drying process. Microparticulated protein has been proven to have improved foaming and emulsifying properties, water and oil absorption capacities and formed long-term stable water dispersions. This work was supported by the research grants TH03010019 of the Technology Agency of the Czech Republic.

Keywords: carbon dioxide-assisted spray nebulization drying, canola seed, hemp seed, microparticulated proteins

Procedia PDF Downloads 138