Search results for: microstructure of weldment

Authors: Sara Khamseh, Kambiz Javanruee, Hamid Khorsand

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Plenty of metallic materials are used for biomedical applications like hip joints and screws. Besides, it is reported that metal platforms such as stainless steel show significant deterioration because of wear and friction. The surface of metal substrates has been coated with a variety of multicomponent coatings to prevail these problems. The carbon-based multicomponent coatings such as metal-added amorphous carbon and diamond coatings are crucially important because of their remarkable tribological performance and chemical stability. In the current study, H-D contained Nb: (a-C) multicomponent coatings (H-D: hexagonal diamond, a-C: amorphous carbon) coated on A 304 steel substrates using an unbalanced magnetron (UBM) sputtering system. The effects of Nb and H-D content and ID/IG ratio on microstructure, mechanical and tribological characteristics of (Nb: H-D: a-C) composite coatings were investigated. The results of Raman spectroscopy represented that a-C phase with a Graphite-like structure (GLC with high value of sp2 carbon bonding) is formed, and its domain size increased with increasing Nb content of the coatings. Moreover, the Nb played a catalyst for the formation of the H-D phase. The nanoindentation hardness value of the coatings ranged between ~17 to ~35 GPa and (Nb: H-D: a-C) composite coatings with more H-D content represented higher hardness and plasticity index. It seems that the existence of extra-hard H-D particles straightly increased hardness. The tribological performance of the coatings was evaluated using the pin-on-disc method under the wet environment of SBF (Simulated Body Fluid). The COF value of the (Nb: H-D: a-C) coatings decreased with an increasing ID/IG ratio. The lower coefficient of friction is a result of the lamelliform array of graphitic domains. Also, the wear rate of the coatings decreased with increasing H-D content of the coatings. Based on the literature, a-C coatings with high hardness and H3/E2 ratio represent lower wear rates and better tribological performance. According to the nanoindentation analysis, hardness and H3/E2 ratio of (Nb: H-D: a-C) multicomponent coatings increased with increasing H-D content, which in turn decreased the wear rate of the coatings. The mechanical and tribological potency of (Nb: H-D: a-C) composite coatings on A 304 steel substrates paved the way for the development of innovative advanced coatings to ameliorate the performance of A 304 steel for biomedical applications.

Keywords: COF, mechanical properties, (Nb: H-D: a-C) coatings, wear rate

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Authors: Li Yang, Yang Song, Martin Y. M. Chiang

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Objective: To experimentally substantiate the micromechanical compatibility between cell and scaffold, in the regenerative medicine approach for restoring bone volume, is essential for phenotypic transitions Methods: Through nanotechnology and electrospinning process, nanofibrous scaffolds were fabricated to host dental follicle stem cells (DFSCs). Blends (50:50) of polycaprolactone (PCL) and silk fibroin (SF), mixed with various content of cellulose nanocrystals (CNC, up to 5% in weight), were electrospun to prepare nanofibrous scaffolds with heterogeneous microstructure in terms of fiber size. Colloidal probe atomic force microscopy (AFM) and conventional uniaxial tensile tests measured the scaffold stiffness at the micro-and macro-scale, respectively. The cell elastic modulus and cell-scaffold adhesive interaction (i.e., a chemical function) were examined through single-cell force spectroscopy using AFM. The quantitative reverse transcription-polymerase chain reaction (qRT-PCR) was used to determine if the mechanotransduction signal (i.e., Yap1, Wwr2, Rac1, MAPK8, Ptk2 and Wnt5a) is upregulated by the scaffold stiffness at the micro-scale (cellular scale). Results: The presence of CNC produces fibrous scaffolds with a bimodal distribution of fiber diameter. This structural heterogeneity, which is CNC-composition dependent, remarkably modulates the mechanical functionality of scaffolds at microscale and macroscale simultaneously, but not the chemical functionality (i.e., only a single material property is varied). In in vitro tests, the osteogenic differentiation and gene expression associated with mechano-sensitive cell markers correlate to the degree of micromechanical compatibility between DFSCs and the scaffold. Conclusion: Cells require compliant scaffolds to encourage energetically favorable interactions for mechanotransduction, which are converted into changes in cellular biochemistry to direct the phenotypic evolution. The micromechanical compatibility is indeed important to the efficacy of regenerative medicine.

Keywords: phenotype transition, scaffold stiffness, electrospinning, cellulose nanocrystals, single-cell force spectroscopy

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Authors: Dounya Barrit, Ming-Chun Tang, Hoang Dang, Kai Wang, Detlef-M. Smilgies, Aram Amassian

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Several deposition methods have been developed for perovskite film preparation. The one-step spin-coating process has emerged as a more popular option thanks to its ability to produce films of different compositions, including mixed cation and mixed halide perovskites, which can stabilize the perovskite phase and produce phases with desired band gap. The two-step method, however, is not understood in great detail. There is a significant need and opportunity to adopt the two-step process toward mixed cation and mixed halide perovskites, but this requires deeper understanding of the two-step conversion process, for instance when using different cations and mixtures thereof, to produce high-quality perovskite films with uniform composition. In this work, we demonstrate using in situ investigations that the conversion of PbI₂ to perovskite is largely dictated by the state of the PbI₂ precursor film in terms of its solvated state. Using time-resolved grazing incidence wide-angle X-Ray scattering (GIWAXS) measurements during spin coating of PbI₂ from a DMF (Dimethylformamide) solution we show the film formation to be a sol-gel process involving three PbI₂-DMF solvate complexes: disordered precursor (P₀), ordered precursor (P₁, P₂) prior to PbI₂ formation at room temperature after 5 minutes. The ordered solvates are highly metastable and eventually disappear, but we show that performing conversion from P₀, P₁, P₂ or PbI₂ can lead to very different conversion behaviors and outcomes. We compare conversion behaviors by using MAI (Methylammonium iodide), FAI (Formamidinium Iodide) and mixtures of these cations, and show that conversion can occur spontaneously and quite rapidly at room temperature without requiring further thermal annealing. We confirm this by demonstrating improvements in the morphology and microstructure of the resulting perovskite films, using techniques such as in situ quartz crystal microbalance with dissipation monitoring, SEM and XRD.

Keywords: in situ GIWAXS, lead iodide, mixed cation, perovskite solar cell, sol-gel process, solvate phase

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Authors: S. Varnagiris, M. Urbonavicius, S. Tuckute, M. Lelis, K. Bockute

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Amongst many water purification techniques, TiO₂ photocatalysis is recognized as one of the most promising sustainable methods. It is known that for photocatalytical applications anatase is the most suitable TiO₂ phase, however heterojunction of anatase/rutile phases could improve the photocatalytical activity of TiO₂ even further. Despite the relative simplicity of TiO₂ different synthesis methods lead to the highly dispersed crystal phases and photocatalytic activity of the corresponding samples. Accordingly, suggestions and investigations of various innovative methods of TiO₂ synthesis are still needed. In this work structural and photocatalytical properties of TiO₂ films deposited by the unconventional method of simultaneous co-sputtering from two magnetrons powered by pulsed-Direct Current (pDC) and Radio Frequency (RF) power sources with negative bias voltage have been studied. More specifically, TiO₂ film thickness, microstructure, surface roughness, crystal structure, optical transmittance and photocatalytical properties were investigated by profilometer, scanning electron microscope, atomic force microscope, X-ray diffractometer and UV-Vis spectrophotometer respectively. The proposed unconventional two magnetron co-sputtering based TiO₂ film formation method showed very promising results for crystalline TiO₂ film formation while keeping process temperatures below 100 °C. XRD analysis revealed that by using proper combination of power source type and bias voltage various TiO₂ phases (amorphous, anatase, rutile or their mixture) can be synthesized selectively. Moreover, strong dependency between power source type and surface roughness, as well as between the bias voltage and band gap value of TiO₂ films was observed. Interestingly, TiO₂ films deposited by two magnetron co-sputtering without bias voltage had one of the highest band gap values between the investigated films but its photocatalytic activity was superior compared to all other samples. It is suggested that this is due to the dominating nanocrystalline anatase phase with various exposed surfaces including photocatalytically the most active {001}.

Keywords: films, magnetron co-sputtering, photocatalysis, TiO₂

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Authors: Evangelia Tsampali, Evangelos Yfantidis, Andreas Ioakim, Maria Stefanidou

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The purpose of this paper is the characterization of the effects of crystalline admixtures on concrete. Crystallites, aided by the presence of humidity, form idiomorphic crystals that block cracks and pores resulting in reduced porosity. In this project, two types of crystallines have been employed. The hydrophilic nature of crystalline admixtures helps the components to react with water and cement particles in the concrete to form calcium silicate hydrates and pore-blocking precipitates in the existing micro-cracks and capillaries. The underlying mechanism relies on the formation of calcium silicate hydrates and the resulting deposits of these crystals become integrally bound with the hydrated cement paste. The crystalline admixtures continue to activate throughout the life of the composite material when in the presence of moisture entering the concrete through hairline cracks, sealing additional gaps. The resulting concrete exhibits significantly increased resistance to water penetration under stress. Admixtures of calcium aluminates can also contribute to this healing mechanism in the same manner. However, this contribution is negligible compared to the calcium silicate hydrates due to the abundance of the latter. These crystalline deposits occur throughout the concrete volume and are a permanent part of the concrete mass. High-performance fibre reinforced cementitious composite (HPFRCC) were produced in the laboratory. The specimens were exposed in three healing conditions: water immersion until testing at 15 °C, sea water immersion until testing at 15 °C, and wet/dry cycles (immersion in tap water for 3 days and drying for 4 days). Specimens were pre-cracked at 28 days, and the achieved cracks width were in the range of 0.10–0.50 mm. Furthermore, microstructure observations and Ultrasonic Pulse Velocity tests have been conducted. Based on the outcomes, self-healing related indicators have also been defined. The results show almost perfect healing capability for specimens healed under seawater, better than for specimens healed in water while inadequate for the wet/dry exposure in both of the crystalline types.

Keywords: autogenous self-healing, concrete, crystalline admixtures, ultrasonic pulse velocity test

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Authors: A. M. Khourshid, I. Sabry

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Friction Stir Welding (FSW), a solid state joining technique, is widely being used for joining Al alloys for aerospace, marine automotive and many other applications of commercial importance. FSW were carried out using a vertical milling machine on Al 5083 alloy pipe. These pipe sections are relatively small in diameter, 5mm, and relatively thin walled, 2 mm. In this study, 5083 aluminum alloy pipe were welded as similar alloy joints using (FSW) process in order to investigate mechanical and microstructural properties .rotation speed 1400 r.p.m and weld speed 10,40,70 mm/min. In order to investigate the effect of welding speeds on mechanical properties, metallographic and mechanical tests were carried out on the welded areas. Vickers hardness profile and tensile tests of the joints as a metallurgical feasibility of friction stir welding for joining Al 6061 aluminum alloy welding was performed on pipe with different thickness 2, 3 and 4 mm,five rotational speeds (485,710,910,1120 and 1400) rpm and a traverse speed (4, 8 and 10)mm/min was applied. This work focuses on two methods such as artificial neural networks using software (pythia) and response surface methodology (RSM) to predict the tensile strength, the percentage of elongation and hardness of friction stir welded 6061 aluminum alloy. An artificial neural network (ANN) model was developed for the analysis of the friction stir welding parameters of 6061 pipe. The tensile strength, the percentage of elongation and hardness of weld joints were predicted by taking the parameters Tool rotation speed, material thickness and travel speed as a function. A comparison was made between measured and predicted data. Response surface methodology (RSM) also developed and the values obtained for the response Tensile strengths, the percentage of elongation and hardness are compared with measured values. The effect of FSW process parameter on mechanical properties of 6061 aluminum alloy has been analyzed in detail.

Keywords: friction stir welding (FSW), al alloys, mechanical properties, microstructure

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Authors: Rekha M. Y., Punith Kumar, Anshul Kamboj, Chandan Srivastava

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Coatings plays an important role in providing protection for a substrate and in improving the surface quality. Graphene/graphene oxide (GO) using in coating systems provides an environmental friendly solution towards protection against corrosion. Issues such as, lack of scale, high cost, low quality limits the practical application of graphene/GO as corrosion resistant coating material. One other way to employ these materials for corrosion protection is to incorporate them into coatings that are conventionally used for corrosion protection. Due to the extraordinary properties of graphene/GO, it has been demonstrated that the coatings containing graphene/GO are more corrosion resistant than pure metal/alloy coatings. In the present work, Cr-graphene and SnZn-GO composite coatings were investigated in enhancing the corrosion resistant property when compared to pure Cr coating and pure SnZn coating respectively. All the coatings were electrodeposited over mild-steel substrate. Graphene and GO were synthesized by electrochemical exfoliation method and modified Hummers’ method respectively. In Cr coatings, the microstructural study revealed that the addition of formic acid in the coatings reduced the number of cracks in the coatings. Further addition of graphene in Cr coating enhanced the Cr coating’s morphology. Chemically synthesized ZnO nanoparticles were also embedded in the as-deposited Cr and Cr-graphene coatings to enhance the adhesion of the coating, to improve the surface finish and to increase the corrosion resistant property of the coatings. Diffraction analysis revealed that the addition of graphene also altered the texture of the Cr coatings. In SnZn alloy coatings, the morphological and topographical characterization revealed that the relative smoothness and compactness of the coatings increased with increase in the addition of GO in the coatings. The microstructural investigation revealed large-scale segregation of Zn-rich and Sn-rich phases in the pure SnZn coating. However, in SnZn-GO composite coating the uniform distribution of Zn phase in the Sn-rich matrix was observed. This distribution caused the early and uniform formation of ZnO, which is the corrosion product, yielding better corrosion resistance for the SnZn-GO composite coatings as compared to pure SnZn coating. A significant improvement in corrosion resistance in terms of reduction in corrosion current and corrosion rate and increase in the polarization resistance was observed in Cr coating containing graphene and in SnZn coatings containing GO.

Keywords: coatings, corrosion, electrodeposition, graphene, graphene-oxide

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Authors: Hanaa A. Al-Gaoudi, Hassan Ebeid

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The research investigates the materials and processes used in the manufacturing of an Egyptian polychrome cartonnage mummy mask with the aim of dating this object and establishing trade patterns of certain materials that were used and available at the time of ancient Egypt. This anonymous-source object was held in the basement storage of the Egyptian Museum in Cairo (EMC) and has never been on display. Furthermore, there is no information available regarding its owner, provenance, date, and even the time of its possession by the museum. Moreover, the object is in a very poor condition where almost two-thirds of the mask was bent and has never received any previous conservation treatment. This research has utilized well-established multi-analytical methods to identify the considerable diversity of materials that have been used in the manufacturing of this object. These methods include Computed Tomography Scan (CT scan) to acquire detailed pictures of the inside physical structure and condition of the bended layers. Dino-Lite portable digital microscope, scanning electron microscopy with energy dispersive X-ray spectrometer (SEM-EDX), and the non-invasive imaging technique of multispectral imaging (MSI) to obtain information about the physical characteristics and condition of the painted layers and to examine the microstructure of the materials. Portable XRF Spectrometer (PXRF) and X-Ray powder diffraction (XRD) to identify mineral phases and the bulk element composition in the gilded layer, ground, and pigments; Fourier-transform infrared (FTIR) to identify organic compounds and their molecular characterization; accelerator mass spectrometry (AMS 14C) to date the object. Preliminary results suggest that there are no human remains inside the object, and the textile support is linen fibres with tabby weave 1/1 and these fibres are in a very bad condition. Several pigments have been identified, such as Egyptian blue, Magnetite, Egyptian green frit, Hematite, Calcite, and Cinnabar; moreover, the gilded layers are pure gold and the binding media in the pigments is Arabic gum and animal glue in the textile support layer.

Keywords: analytical methods, Egyptian museum, mummy mask, pigments, textile

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Authors: Merzak Laribi, Abdelmadjid Kasser

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Thermal spraying processes are widely used to produce coatings on original constructions as well as in repair and maintenance of long standing structures. A lot of efforts forwarding to develop thermal spray coatings technology have been focused on improving mechanical characteristics, minimizing residual stress level and reducing porosity of the coatings. The specific aim of this paper is to determine either residual stresses distribution or wear resistance of stainless steel coating thermally sprayed on a carbon steel substrate. Internal stresses determination was performed using an extensometric method in combination with a simultaneous progressive electrolytic polishing. The procedure consists of measuring micro-deformations using a bi-directional extensometric gauges glued on the substrate side of the materials. Very thin layers of the deposits are removed by electrochemical polishing across the sample surface. Micro-deformations are instantaneously measured, leading to residual stresses calculation after each removal. Wear resistance of the coating has been determined using a ball-on-plate tribometer. Friction coefficient is instantaneously measured during the tribological test. Attention was particularly focused on the influence of a post-annealing at 850 °C for one hour in vacuum either on the residual stresses distribution or on the wear resistance behavior under specific wear and lubrication conditions. The obtained results showed that the microstructure of the obtained arc sprayed stainless steel coating is classical. It is homogeneous and contains un-melted particles, metallic oxides and also pores and micro-cracks. The internal stresses are in compression in the coating. They are more or less scattered between -50 and -270 MPa on the surface and decreased more at the interface. The value at the surface of the substrate is about –700 MPa, partially due to the molten particles impact with the substrate. The post annealing has reduced the residual stresses in both coating and surface of the steel substrate so that the hole material becomes more relaxed. Friction coefficient has an average value of 0.3 and 0.4 respectively for non annealed and annealed specimen. It is rather oil lubrication which is really benefit so that friction coefficient is decreased to about 0.06.

Keywords: residual stresses, wear resistance, stainless steel, coating, thermal spraying, annealing, lubrication

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Authors: Huanru Wang, Jianzhun Jiang

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At present, the preparation of the catalyst by carbon carrier is one of the improvement directions of the C₂ pre-hydrogenation catalyst. Carbon materials can be prepared from coal direct liquefaction residues, coconut shells, biomass, etc., and the pore structure of carbon carrier materials can be adjusted through the preparation process; at high temperatures, the carbon carrier itself also shows certain catalytic activity. Therefore, this paper mainly selected typical activated carbon and coconut shell carbon as carbon carrier materials, studied their microstructure and surface properties, prepared a series of carbon-based catalysts loaded with Pd, and investigated the effects of the content of promoter Ag and the concentration of reductant on the structure and performance of the catalyst and its catalytic performance for the pre hydrogenation of C₂. In this paper, the carbon supports from two sources and the catalysts prepared by them were characterized in detail. The results showed that the morphology and structure of different supports and the performance of the catalysts prepared were also obviously different. The catalyst supported on coconut shell carbon has a small specific surface area and large pore diameter. The catalyst supported on activated carbon has a large specific surface area and rich pore structure. The active carbon support is mainly a mixture of amorphous graphite and microcrystalline graphite. For the catalyst prepared with coconut shell carbon as the carrier, the sample is very uneven, and its specific surface area and pore volume are irregular. Compared with coconut shell carbon, activated carbon is more suitable as the carrier of the C₂ hydrogenation catalyst. The conversion of acetylene, methyl acetylene, and butadiene decreased, and the ethylene selectivity increased after Ag was added to the supported Pd catalyst. When the amount of promoter Ag is 0.01-0.015%, the catalyst has relatively good catalytic performance. Ag and Pd form an alloying effect, thus reducing the effective demand for Ag. The Pd Ag ratio is the key factor affecting the catalytic performance. When the addition amount of Ag is 0.01-0.015%, the dispersion of Pd on the carbon support surface can be significantly improved, and the size of active particles can be reduced. The Pd Ag ratio is the main factor in improving the selectivity of the catalyst. When the additional amount of sodium formate is 1%, the catalyst prepared has both high acetylene conversion and high ethylene selectivity.

Keywords: C₂ hydrogenation, activated carbon, Ag promoter, Pd catalysts

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Authors: Mohammad M. Khan, Gajendra Dixit

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Partially lubricated sliding wear behaviour of a zinc-based alloy reinforced with 10wt% SiC particles has been studied as a function of applied load and solid lubricant particle size and has been compared with that of matrix alloy and conventionally used grey cast iron. The wear tests were conducted at the sliding velocities of 2.1m/sec in various partial lubricated conditions using pin on disc machine as per ASTM G-99-05. Base oil (SAE 20W-40) or mixture of the base oil with 5wt% graphite of particle sizes (7-10 µm) and (100 µm) were used for creating lubricated conditions. The matrix alloy revealed primary dendrites of a and eutectoid a + h and Î phases in the Inter dendritic regions. Similar microstructure has been depicted by the composite with an additional presence of the dispersoid SiC particles. In the case of cast iron, flakes of graphite were observed in the matrix; the latter comprised of (majority of) pearlite and (limited quantity of) ferrite. Results show a large improvement in wear resistance of the zinc-based alloy after reinforcement with SiC particles. The cast iron shows intermediate response between the matrix alloy and composite. The solid lubrication improved the wear resistance and friction behaviour of both the reinforced and base alloy. Moreover, minimum wear rate is obtained in oil+ 5wt % graphite (7-10 µm) lubricated environment for the matrix alloy and composite while for cast iron addition of solid lubricant increases the wear rate and minimum wear rate is obtained in case of oil lubricated environment. The cast iron experienced higher frictional heating than the matrix alloy and composite in all the cases especially at higher load condition. As far as friction coefficient is concerned, a mixed trend of behaviour was noted. The wear rate and frictional heating increased with load while friction coefficient was affected in an opposite manner. Test duration influenced the frictional heating and friction coefficient of the samples in a mixed manner.

Keywords: solid lubricant, sliding wear, grey cast iron, zinc based metal matrix composites

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Authors: Martin Tazky, Rudolf Hela, Lucia Osuska, Petr Novosad

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Concrete’s volumetric changes are natural process caused by silicate minerals’ hydration. These changes can lead to cracking and subsequent destruction of cementitious material’s matrix. In most cases, cracks can be assessed as a negative effect of hydration, and in all cases, they lead to an acceleration of degradation processes. Preventing the formation of these cracks is, therefore, the main effort. Once of the possibility how to eliminate this natural concrete shrinkage process is by using different types of dispersed reinforcement. For this application of concrete shrinking, steel and polymer reinforcement are preferably used. Despite ordinarily used reinforcement in concrete to eliminate shrinkage it is possible to look at this specific problematic from the beginning by itself concrete mix composition. There are many secondary raw materials, which are helpful in reduction of hydration heat and also with shrinkage of concrete during curing. The new science shows the possibilities of shrinkage reduction also by the controlled formation of hydration products, which could act by itself morphology as a traditionally used dispersed reinforcement. This contribution deals with the possibility of controlled formation of mono- and tri-sulfate which are considered like degradation minerals. Mono- and tri- sulfate's controlled formation in a cementitious composite can be classified as a self-healing ability. Its crystal’s growth acts directly against the shrinking tension – this reduces the risk of cracks development. Controlled formation means that these crystals start to grow in the fresh state of the material (e.g. concrete) but stop right before it could cause any damage to the hardened material. Waste materials with the suitable chemical composition are very attractive precursors because of their added value in the form of landscape pollution’s reduction and, of course, low cost. In this experiment, the possibilities of using the fly ash from fluidized bed combustion as a mono- and tri-sulphate formation additive were investigated. The experiment itself was conducted on cement paste and concrete and specimens were subjected to a thorough analysis of physicomechanical properties as well as microstructure from the moment of mixing up to 180 days. In cement composites, were monitored the process of hydration and shrinkage. In a mixture with the used admixture of fluidized bed combustion fly ash, possible failures were specified by electronic microscopy and dynamic modulus of elasticity. The results of experiments show the possibility of shrinkage concrete reduction without using traditionally dispersed reinforcement.

Keywords: shrinkage, monosulphates, trisulphates, self-healing, fluidized fly ash

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Authors: Qing Liu, Jean-fabien Capsal, Claude Richard

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In this current contribution, authors are dedicated to investigate influence of the crystal lamellae orientation on electromechanical behaviors of relaxor ferroelectric Poly (vinylidene fluoride –trifluoroethylene -chlorotrifluoroethylene) (P(VDF-TrFE-CTFE)) films by control of polymer microstructure, aiming to picture the full map of structure-property relationship. In order to define their crystal orientation films, terpolymer films were fabricated by solution-casting, stretching and hot-pressing process. Differential scanning calorimetry, impedance analyzer, and tensile strength techniques were employed to characterize crystallographic parameters, dielectric permittivity, and elastic Young’s modulus respectively. In addition, large electrical induced out-of-plane electrostrictive strain was obtained by cantilever beam mode. Consequently, as-casted pristine films exhibited surprisingly high electrostrictive strain 0.1774% due to considerably small value of elastic Young’s modulus although relatively low dielectric permittivity. Such reasons contributed to large mechanical elastic energy density. Instead, due to 2 folds increase of elastic Young’s modulus and less than 50% augmentation of dielectric constant, fully-crystallized film showed weak electrostrictive behavior and mechanical energy density as well. And subjected to mechanical stretching process, Film C exhibited stronger dielectric constant and out-performed electrostrictive strain over Film B because edge-on crystal lamellae orientation induced by uniaxially mechanical stretch. Hot-press films were compared in term of cooling rate. Rather large electrostrictive strain of 0.2788% for hot-pressed Film D in quenching process was observed although its dielectric permittivity equivalent to that of pristine as-casted Film A, showing highest mechanical elastic energy density value of 359.5 J/m^3. In hot-press cooling process, dielectric permittivity of Film E saw values at 48.8 concomitant with ca.100% increase of Young’s modulus. Films with intermediate mechanical energy density were obtained.

Keywords: crystal orientation, electrostroctive strain, mechanical energy density, permittivity, relaxor ferroelectric

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Authors: I. Sinnarasa, Y. Thimont, L. Presmanes, A. Barnabé

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The thermoelectricity is a promising technique to overcome the issues in recovering waste heat to electricity without using moving parts. In fact, the thermoelectric (TE) effect defines as the conversion of a temperature gradient directly into electricity and vice versa. To optimize TE materials, the power factor (PF = σS² where σ is electrical conductivity and S is Seebeck coefficient) must be increased by adjusting the carrier concentration, and/or the lattice thermal conductivity Kₜₕ must be reduced by introducing scattering centers with point defects, interfaces, and nanostructuration. The PF does not show the advantages of the thin film because it does not take into account the thermal conductivity. In general, the thermal conductivity of the thin film is lower than the bulk material due to their microstructure and increasing scattering effects with decreasing thickness. Delafossite type oxides CuᴵMᴵᴵᴵO₂ received main attention for their optoelectronic properties as a p-type semiconductor they exhibit also interesting thermoelectric (TE) properties due to their high electrical conductivity and their stability in room atmosphere. As there are few proper studies on the TE properties of Mg-doped CuCrO₂ thin films, we have investigated, the influence of the annealing temperature on the electrical conductivity and the Seebeck coefficient of Mg-doped CuCrO₂ thin films and calculated the PF in the temperature range from 40 °C to 220 °C. For it, we have deposited Mg-doped CuCrO₂ thin films on fused silica substrates by RF magnetron sputtering. This study was carried out on 300 nm thin films. The as-deposited Mg doped CuCrO₂ thin films have been annealed at different temperatures (from 450 to 650 °C) under primary vacuum. Electrical conductivity and Seebeck coefficient of the thin films have been measured from 40 to 220 °C. The highest electrical conductivity of 0.60 S.cm⁻¹ with a Seebeck coefficient of +329 µV.K⁻¹ at 40 °C have been obtained for the sample annealed at 550 °C. The calculated power factor of optimized CuCrO₂:Mg thin film was 6 µW.m⁻¹K⁻² at 40 °C. Due to the constant Seebeck coefficient and the increasing electrical conductivity with temperature it reached 38 µW.m⁻¹K⁻² at 220 °C that was a quite good result for an oxide thin film. Moreover, the degenerate behavior and the hopping mechanism of CuCrO₂:Mg thin film were elucidated. Their high and constant Seebeck coefficient in temperature and their stability in room atmosphere could be a great advantage for an application of this material in a high accuracy temperature measurement devices.

Keywords: thermoelectric, oxides, delafossite, thin film, power factor, degenerated semiconductor, hopping mode

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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. Busuioc, I. Stancu, A. Nicoara, A. Zamfirescu, A. Evanghelidis

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The field of tissue engineering has expanded its potential due to the use of composite biomaterials belonging to increasingly complex systems, leading to bone substitutes with properties that are continuously improving to meet the patient's specific needs. Furthermore, the development of biomaterials based on ceramic and polymeric phases is an unlimited resource for future scientific research, with the final aim of restoring the original tissue functionality. Thus, in the first stage, composite scaffolds based on polycaprolactone (PCL) or polylactic acid (PLA) and inorganic powders were prepared by employing the electrospinning technique. The targeted powders were: commercial and laboratory synthesized hydroxyapatite (HAp), as well as barium titanate (BT). By controlling the concentration of the powder within the precursor solution, together with the processing parameters, different types of three-dimensional architectures were achieved. In the second stage, both the mineral powders and hybrid composites were investigated in terms of composition, crystalline structure, and microstructure so that to demonstrate their suitability for tissue engineering applications. Regarding the scaffolds, these were proven to be homogeneous on large areas and loaded with mineral particles in different proportions. The biological assays demonstrated that the addition of inorganic powders leads to modified responses in the presence of simulated body fluid (SBF) or cell cultures. Through SBF immersion, the biodegradability coupled with bioactivity were highlighted, with fiber fragmentation and surface degradation, as well as apatite layer formation within the testing period. Moreover, the final composites represent supports accepted by the cells, favoring implant integration. Concluding, the purposed fibrous materials based on bioresorbable polymers and mineral powders, produced by the electrospinning technique, represent candidates with considerable potential in the field of tissue engineering. Future improvements can be attained by optimizing the synthesis process or by simultaneous incorporation of multiple inorganic phases with well-defined biological action in order to fabricate multifunctional composites.

Keywords: barium titanate, electrospinning, fibre networks, hydroxyapatite, smart scaffolds

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Authors: M.St. Węglowski, D. Miara, S. Błacha, J. Dworak, J. Rykała, K. Kwieciński, J. Pikuła, G. Ziobro, A. Szafron, P. Zimierska-Nowak, M. Richert, P. Noga

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In the paper the results of welding of car’s air-conditioning elements are presented. These systems based on, mainly, the environmental unfriendly refrigerants. Thus, the producers of cars will have to stop using traditional refrigerant and to change it to carbon dioxide (R744). This refrigerant is environmental friendly. However, it should be noted that the air condition system working with R744 refrigerant operates at high temperature (up to 150 °C) and high pressure (up to 130 bar). These two parameters are much higher than for other refrigerants. Thus new materials, design as well as joining technologies are strongly needed for these systems. AISI 304 and 316L steels as well as aluminium alloys 5xxx are ranked among the prospective materials. As a joining process laser welding, plasma welding, electron beam welding as well as high rotary friction welding can be applied. In the study, the metallographic examination based on light microscopy as well as SEM was applied to estimate the quality of welded joints. The analysis of welding was supported by numerical modelling based on Sysweld software. The results indicated that using laser, plasma and electron beam welding, it is possible to obtain proper quality of welds in stainless steel. Moreover, high rotary friction welding allows to guarantee the metallic continuity in the aluminium welded area. The metallographic examination revealed that the grain growth in the heat affected zone (HAZ) in laser and electron beam welded joints were not observed. It is due to low heat input and short welding time. The grain growth and subgrains can be observed at room temperature when the solidification mode is austenitic. This caused low microstructural changes during solidification. The columnar grain structure was found in the weld metal. Meanwhile, the equiaxed grains were detected in the interface. The numerical modelling of laser welding process allowed to estimate the temperature profile in the welded joint as well as predicts the dimensions of welds. The agreement between FEM analysis and experimental data was achieved.  

Keywords: car’s air–conditioning, microstructure, numerical modelling, welding

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Authors: Sajad A. Rather, F. A. Masoodi, Rehana Akhter, S. M. Wani, Adil Gani

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Modern trend towards convenience foods has resulted in increased production and consumption of restructured meat products and are of great importance to the meat industry. In meat products fat plays an important role in cooking properties, texture & sensory scores, however, high fat contents in particular animal fats provide high amounts of saturated fatty acids and cholesterol and are associated with several types of non communicable diseases such as obesity, hypertension and coronary heart diseases. Thus, fat reduction has generally been seen as an important strategy to produce healthier meat products. This study examined the effects of reducing fat level from 20% to 10% and substituting mutton back fat with guar gum (0.5%, 1% & 1.5%) on cooking properties, proximate composition, lipid and protein oxidation, texture, microstructure and sensory characteristics of goshtaba- a traditional meat product of J & K, India were investigated and compared with high fat counterparts. Reduced- fat goshtaba samples containing guar gum had significantly (p ≤ 0.05) higher yield, less shrinkage, more moisture retention and more protein content than the control sample. TBARs and protein oxidation (carbonyl content) values of the control was significantly (p ≤ 0.05) higher than reduced fat goshtaba samples and showed a positive correlation between lipid and protein oxidation. Hardness, gumminess & chewiness of the control (20%) were significantly higher than reduced fat goshtaba samples. Microstructural differences were significant (p ≤ 0.05) between control and treated samples due to an increased moisture content in the reduced fat samples. Sensory evaluation showed significant (p ≤ 0.05) reduction in texture, flavour and overall acceptability scores of treatment products; however the scores for 0.5% and 1% treated samples were in the range of acceptability. Guar gum may also be used as a source of soluble dietary fibre in food products and a number of clinical studies have shown a reduction in postprandial glycemia and insulinemia on consumption of guar gum, with the mechanism being attributed to an increased transit time in the stomach and small intestine, which may have been due to the viscosity of the meal hindering the access of glucose to the epithelium.

Keywords: goshtaba, guar gum, traditional, fat reduction, acceptability

Procedia PDF Downloads 259

Authors: B. V. Feujofack Kemda, N. Barka, M. Jahazi, D. Osmani

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Automobile manufacturers are constantly seeking means to reduce the weight of car bodies. The usage of several steel grades in auto body assembling has been found to be a good technique to enlighten vehicles weight. This few years, the usage of dual phase (DP) steels, transformation induced plasticity (TRIP) steels and boron steels in some parts of the auto body have become a necessity because of their lightweight. However, these steels are martensitic, when they undergo a fast heat treatment, the resultant microstructure is essential, made of martensite. Resistance spot welding (RSW), one of the most used techniques in assembling auto bodies, becomes problematic in the case of these steels. RSW being indeed a process were steel is heated and cooled in a very short period of time, the resulting weld nugget is mostly fully martensitic, especially in the case of DP, TRIP and boron steels but that also holds for plain carbon steels as AISI 1010 grade which is extensively used in auto body inner parts. Martensite in its turn must be avoided as most as possible when welding steel because it is the principal source of brittleness and it weakens weld nugget. Thus, this work aims to find a mean to reduce martensite fraction in weld nugget when using RSW for assembling. The prediction of phase transformation kinetics during RSW has been done. That phase transformation kinetics prediction has been made possible through the modelling of the whole welding process, and a technique called post weld heat treatment (PWHT) have been applied in order to reduce martensite fraction in the weld nugget. Simulation has been performed for AISI 1010 grade, and results show that the application of PWHT leads to the formation of not only martensite but also ferrite, bainite and pearlite during the cooling of weld nugget. Welding experiments have been done in parallel and micrographic analyses show the presence of several phases in the weld nugget. Experimental weld geometry and phase proportions are in good agreement with simulation results, showing here the validity of the model.

Keywords: resistance spot welding, AISI 1010, modeling, post weld heat treatment, phase transformation, kinetics

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Authors: Chih-Chung Huang, Po-Hsun Peng

Abstract:

Ultrasound transient elastography has become a valuable tool for many clinical diagnoses, such as liver diseases and breast cancer. The pathological tissue can be distinguished by elastography due to its stiffness is different from surrounding normal tissues. An ultrafast frame rate of ultrasound imaging is needed for transient elastography modality. The elastography obtained in the ultrafast system suffers from a low quality for resolution, and affects the robustness of the transient elastography. In order to overcome these problems, a coherent plane wave compounding technique has been proposed for conventional ultrasound system which the operating frequency is around 3-15 MHz. The purpose of this study is to develop a novel beamforming technique for high frequency ultrasound coherent plane-wave compounding imaging and the simulated results will provide the standards for hardware developments. Plane-wave compounding imaging produces a series of low-resolution images, which fires whole elements of an array transducer in one shot with different inclination angles and receives the echoes by conventional beamforming, and compounds them coherently. Simulations of plane-wave compounding image and focused transmit image were performed using Field II. All images were produced by point spread functions (PSFs) and cyst phantoms with a 64-element linear array working at 35MHz center frequency, 55% bandwidth, and pitch of 0.05 mm. The F number is 1.55 in all the simulations. The simulated results of PSFs and cyst phantom which were obtained using single, 17, 43 angles plane wave transmission (angle of each plane wave is separated by 0.75 degree), and focused transmission. The resolution and contrast of image were improved with the number of angles of firing plane wave. The lateral resolutions for different methods were measured by -10 dB lateral beam width. Comparison of the plane-wave compounding image and focused transmit image, both images exhibited the same lateral resolution of 70 um as 37 angles were performed. The lateral resolution can reach 55 um as the plane-wave was compounded 47 angles. All the results show the potential of using high-frequency plane-wave compound imaging for realizing the elastic properties of the microstructure tissue, such as eye, skin and vessel walls in the future.

Keywords: plane wave imaging, high frequency ultrasound, elastography, beamforming

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Authors: Gulay Oncu Ince, Sibel Karakaya

Abstract:

Food is a worldwide concern. Among the factors that have influences on human health, food, nutrition and life style have been regarded as the most important factors since they can be intervened. While some parts of the world has been faced with food shortages and hence, chronic metabolic diseases, the other part of the world have been emerged from over consumption of food. Both situations can result in shorter life expectancy and represent a major global health problem. Hunger, satiety and appetite sensation form a balance ensures the operation of feeding behavior between food intake and energy consumption. Satiety is one of the approaches that is effective in ensuring weight control and avoid eating more in the postprandial period. By manipulating the microstructure of food macro and micronutrient bioavailability may be increased or reduced. For the food industry appearance, texture, taste structural properties as well as the gastrointestinal tract behavior of the food after the consumption is becoming increasingly important. Also, this behavior has been the subject of several researches in recent years by the scientific community. Numerous studies have been published about changing the food matrix in order to increase expected impacts. In this study, yogurts were enriched with caseinomacropeptide (CMP), whey protein (WP), CMP and sodium alginate (SA), and WP + SA in order to produce goat yogurts having different food matrices. SDS Page profiles of the samples after in vitro digestion and viscosities of the stomach digesta at different share rates were determined. Energy values were 62.11kcal/100 g, 70.27 kcal/100 g, 70.61 kcal/100 g, 71.20 kcal/100 g and 71.67 kcal/100 g for control, CMP added WP added, WP + SA added, and CMP + SA added yogurts respectively. The results of viscosity analysis showed that control yogurt had the lowest viscosity value and this was followed by CMP added, WP added, CMP + SA added and WP + SA added yogurts, respectively. Protein contents of the stomach and duedonal digests of the samples after subjected to two different in vitro digestion methods were changed between 5.34-5.91 mg protein / g sample and 16.93-19.75 mg protein /g of sample, respectively. Viscosity measurements of the stomach digests showed that CMP + SA added yogurt displayed the highest viscosity value in both in vitro digestion methods. There were differences between the protein profiles of the stomach and duedonal digests obtained by two different in vitro digestion methods (p<0.05).

Keywords: caseinomacropeptide, protein profile, whey protein, yogurt

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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: Sami W. Tabsh

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The strength of reinforced concrete depends on the member dimensions and material properties. The properties of concrete and steel materials are not constant but random variables. The variability of concrete strength is due to batching errors, variations in mixing, cement quality uncertainties, differences in the degree of compaction and disparity in curing. Similarly, the variability of steel strength is attributed to the manufacturing process, rolling conditions, characteristics of base material, uncertainties in chemical composition, and the microstructure-property relationships. To account for such uncertainties, codes of practice for reinforced concrete design impose resistance factors to ensure structural reliability over the useful life of the structure. In this investigation, the effects of reductions in concrete and reinforcing steel strengths from the nominal values, beyond those accounted for in the structural design codes, on the structural reliability are assessed. The considered limit states are flexure, shear and axial compression based on the ACI 318-11 structural concrete building code. Structural safety is measured in terms of a reliability index. Probabilistic resistance and load models are compiled from the available literature. The study showed that there is a wide variation in the reliability index for reinforced concrete members designed for flexure, shear or axial compression, especially when the live-to-dead load ratio is low. Furthermore, variations in concrete strength have minor effect on the reliability of beams in flexure, moderate effect on the reliability of beams in shear, and sever effect on the reliability of columns in axial compression. On the other hand, changes in steel yield strength have great effect on the reliability of beams in flexure, moderate effect on the reliability of beams in shear, and mild effect on the reliability of columns in axial compression. Based on the outcome, it can be concluded that the reliability of beams is sensitive to changes in the yield strength of the steel reinforcement, whereas the reliability of columns is sensitive to variations in the concrete strength. Since the embedded target reliability in structural design codes results in lower structural safety in beams than in columns, large reductions in material strengths compromise the structural safety of beams much more than they affect columns.

Keywords: code, flexure, limit states, random variables, reinforced concrete, reliability, reliability index, shear, structural safety

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Authors: Luvindran Sugumaran, Mohd Nashrul Mohd Zubir, Kazi Md Salim Newaz, Tuan Zaharinie Tuan Zahari, Suazlan Mt Aznam, Aiman Mohd Halil

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With the fast growth of integrated circuits and the trend towards making electronic devices smaller, the heat dissipation load of electronic devices has continued to go over the limit. The high heat flux element would not only harm the operation and lifetime of the equipment but would also impede the performance upgrade brought about by the iteration of technological updates, which would have a direct negative impact on the economic and production cost benefits of rising industries. Hence, in high-tech industries like radar, information and communication, electromagnetic power, and aerospace, the development and implementation of effective heat dissipation technologies were urgently required. Pool boiling is favored over other cooling methods because of its capacity to dissipate a high heat flux at a low wall superheat without the usage of mechanical components. Enhancing the pool boiling performance by increasing the heat transfer coefficient via surface modification techniques has received a lot of attention. There are several surface modification methods feasible today, but the stability and durability of surface modification are the greatest priority. Thus, laser machining is an interesting choice for surface modification due to its low production cost, high scalability, and repeatability. In this study, different patterns of laser-processed copper surfaces are fabricated to investigate the nucleate pool boiling heat transfer performance of distilled water. The investigation showed that there is a significant enhancement in the pool boiling heat transfer performance of the laser-processed surface compared to the reference surface due to the notable increase in nucleation frequency and nucleation site density. It was discovered that the heat transfer coefficients increased when both the surface area ratio and the ratio of peak-to-valley height of the microstructure were raised. It is believed that the development of microstructures on the surface as a result of laser processing is the primary factor in the enhancement of heat transfer performance.

Keywords: heat transfer coefficient, laser processing, micro structured surface, pool boiling

Procedia PDF Downloads 63

Authors: Shakti S. Acharya, V. R. R. Medicherla, Rajeev Rawat, Komal Bapna, Deepnarayan Biswas, Khadija Ali, K. Maiti

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The discovery of invar effect in 35% Ni concentration Fe1-xNix alloy has stimulated enormous experimental and theoretical research. Elemental Fe and low Ni concentration Fe1-xNix alloys which possess body centred cubic (bcc) crystal structure at ambient temperature and pressure transform to hexagonally close packed (hcp) phase at around 13 GPa. Magnetic order was found to be absent at 11K for Fe92Ni8 alloy when subjected to a high pressure of 26 GPa. The density functional theoretical calculations predicted substantial hyperfine magnetic fields, but were not observed in Mossbaur spectroscopy. The bulk modulus of fcc Fe1-xNix alloys with Ni concentration more than 35%, is found to be independent of pressure. The magnetic moment of Fe is also found be almost same in these alloys from 4 to 10 GPa pressure. Fe1-xNix alloys exhibit a complex microstructure which is formed by a series of complex phase transformations like martensitic transformation, spinodal decomposition, ordering, mono-tectoid reaction, eutectoid reaction at temperatures below 400°C. Despite the existence of several theoretical models the field is still in its infancy lacking full knowledge about the anomalous properties exhibited by these alloys. Fe1-xNix alloys have been prepared by arc melting the high purity constituent metals in argon ambient. These alloys have annealed at around 3000C in vacuum sealed quartz tube for two days to make the samples homogeneous. These alloys have been structurally characterized by x-ray diffraction and were found to exhibit a transition from bcc to fcc for x > 0.3. Ni 2p core levels of the alloys have been measured using high resolution (0.45 eV) x-ray photoelectron spectroscopy. Ni 2p core level shifts to lower binding energy with respect to that of pure Ni metal giving rise to negative core level shifts (CLSs). Measured CLSs exhibit a linear dependence in fcc region (x > 0.3) and were found to deviate slightly in bcc region (x < 0.3). ESCA potential model fails correlate CLSs with site potentials or charges in metallic alloys. CLSs in these alloys occur mainly due to shift in valence bands with composition due to intra atomic charge redistribution.

Keywords: arc melting, core level shift, ESCA potential model, valence band

Procedia PDF Downloads 359

Authors: Lei Zhao, Yi Song, Tim Dunne, Jiaxiang (Jason) Ren, Wenhan Yue, Lei Yang, Li Wen, Yu Liu

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Fasting dissolving magnesium (DM) alloy technology has contributed significantly to the “Shale Revolution” in oil and gas industry. This application requires DM downhole tools dissolving initially at a slow rate, rapidly accelerating to a high rate after certain period of operation time (typically 8 h to 2 days), a contradicting requirement that can hardly be addressed by traditional Mg alloying or processing itself. Premature disintegration has been broadly reported in downhole DM tool from field trials. To address this issue, “temporary” thin polymers of various formulations are currently coated onto DM surface to delay its initial dissolving. Due to conveying parts, harsh downhole condition, and high dissolving rate of the base material, the current delay coatings relying on pure polymers are found to perform well only at low temperature (typical < 100 ℃) and parts without sharp edges or corners, as severe geometries prevent high quality thin film coatings from forming effectively. In this study, a coating technology combining Plasma Electrolytic Oxide (PEO) coatings with advanced thin film deposition has been developed, which can delay DM complex parts (with sharp corners) in corrosive fluid at 150 ℃ for over 2 days. Synergistic effects between porous hard PEO coating and chemical inert elastic-polymer sealing leads to its delaying dissolution improvement, and strong chemical/physical bonding between these two layers has been found to play essential role. Microstructure of this advanced coating and compatibility between PEO and various polymer selections has been thoroughly investigated and a model is also proposed to explain its delaying performance. This study could not only benefit oil and gas industry to unplug their High Temperature High Pressure (HTHP) unconventional resources inaccessible before, but also potentially provides a technical route for other industries (e.g., bio-medical, automobile, aerospace) where primer anti-corrosive protection on light Mg alloy is highly demanded.

Keywords: dissolvable magnesium, coating, plasma electrolytic oxide, sealer

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Authors: M. Abderrahmane Mograne, Didier Laux, Jean-Yves Ferrandis

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Rheological characterizations of complex liquids like polymer solutions present an important scientific interest for a lot of researchers in many fields as biology, food industry, chemistry. In order to establish master curves (elastic moduli vs frequency) which can give information about microstructure, classical rheometers or viscometers (such as Couette systems) are used. For broadband characterization of the sample, temperature is modified in a very large range leading to equivalent frequency modifications applying the Time Temperature Superposition principle. For many liquids undergoing phase transitions, this approach is not applicable. That is the reason, why the development of broadband spectroscopic methods around room temperature becomes a major concern. In literature many solutions have been proposed but, to our knowledge, there is no experimental bench giving the whole rheological characterization for frequencies about a few Hz (Hertz) to many MHz (Mega Hertz). Consequently, our goal is to investigate in a nondestructive way in very broadband frequency (A few Hz – Hundreds of MHz) rheological properties using longitudinal ultrasonic waves (L waves), a unique experimental bench and a specific container for the liquid: a test tube. More specifically, we aim to estimate the three viscosities (longitudinal, shear and bulk) and the complex elastic moduli (M*, G* and K*) respectively longitudinal, shear and bulk moduli. We have decided to use only L waves conditioned in two ways: bulk L wave in the liquid or guided L waves in the tube test walls. In this paper, we will present first results for very low frequencies using the ultrasonic tracking of a falling ball in the test tube. This will lead to the estimation of shear viscosity from a few mPa.s to a few Pa.s (Pascal second). Corrections due to the small dimensions of the tube will be applied and discussed regarding the size of the falling ball. Then the use of bulk L wave’s propagation in the liquid and the development of a specific signal processing in order to assess longitudinal velocity and attenuation will conduct to the longitudinal viscosity evaluation in the MHz frequency range. At last, the first results concerning the propagation, the generation and the processing of guided compressional waves in the test tube walls will be discussed. All these approaches and results will be compared to standard methods available and already validated in our lab.

Keywords: nondestructive measurement for liquid, piezoelectric transducer, ultrasonic longitudinal waves, viscosities

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Authors: Eun-Soo Lim, Young-Min Kang

Abstract:

M-type Sr-hexaferrite (SrFe₁₂O₁₉) have been studied during the past decades because it is the most utilized materials in permanent magnets due to their low price, outstanding chemical stability, and appropriate hard magnetic properties. Many attempts have been made to improve the intrinsic magnetic properties of M-type Sr-hexaferrites (SrM), such as by improving the saturation magnetization (MS) and crystalline anisotropy by cation substitution. It is well proved that the Ca-La-Co substitutions are one of the most successful approaches, which lead to a significant enhancement in the crystalline anisotropy without reducing MS, and thus the Ca-La-Co-doped SrM have been commercialized in high-grade magnet products. In this research, the effect of respective doping of Ca and La into the SrM lattices were studied with assumptions that these elements could substitute both of Fe and Sr sites. The hexaferrite samples of stoichiometric SrFe₁₂O₁₉ (SrM) and the Ca substituted SrM with formulae of Sr₁₋ₓCaₓFe₁₂Oₐ (x = 0.1, 0.2, 0.3, 0.4) and SrFe₁₂₋ₓCaₓOₐ (x = 0.1, 0.2, 0.3, 0.4), and also La substituted SrM of Sr₁₋ₓLaₓFe₁₂Oₐ (x = 0.1, 0.2, 0.3, 0.4) and SrFe₁₂₋ₓLaₓOₐ (x = 0.1, 0.2, 0.3, 0.4) were prepared by conventional solid state reaction processes. X-ray diffraction (XRD) with a Cu Kα radiation source (λ=0.154056 nm) was used for phase analysis. Microstructural observation was conducted with a field emission scanning electron microscopy (FE-SEM). M-H measurements were performed using a vibrating sample magnetometer (VSM) at 300 K. Almost pure M-type phase could be obtained in the all series of hexaferrites calcined at > 1250 ºC. Small amount of Fe₂O₃ phases were detected in the XRD patterns of Sr₁₋ₓCaₓFe₁₂Oₐ (x = 0.2, 0.3, 0.4) and Sr₁₋ₓLaₓFe₁₂Oₐ (x = 0.1, 0.2, 0.3, 0.4) samples. Also, small amount of unidentified secondary phases without the Fe₂O₃ phase were found in the samples of SrFe₁₂₋ₓCaₓOₐ (x = 0.4) and SrFe₁₂₋ₓLaₓOₐ (x = 0.3, 0.4). Although the Ca substitution (x) into SrM structure did not exhibit a clear tendency in the cell parameter change in both series of samples, Sr₁₋ₓCaₓFe₁₂Oₐ and SrFe₁₂₋ₓCaₓOₐ , the cell volume slightly decreased with doping of Ca in the Sr₁₋ₓCaₓFe₁₂Oₐ samples and increased in the SrFe₁₂₋ₓCaₓOₐ samples. Considering relative ion sizes between Sr²⁺ (0.113 nm), Ca²⁺ (0.099 nm), Fe³⁺ (0.064 nm), these results imply that the Ca substitutes both of Sr and Fe in the SrM. A clear tendency of cell parameter change was observed in case of La substitution into Sr site of SrM ( Sr₁₋ₓLaₓFe₁₂Oₐ); the cell volume decreased with increase of x. It is owing to the similar but smaller ion size of La³⁺ (0.106 nm) than that of Sr²⁺. In case of SrFe₁₂₋ₓLaₓOₐ, the cell volume first decreased at x = 0.1 and then remained almost constant with increase of x from 0.2 to 0.4. These results mean that La only substitutes Sr site in the SrM structure. Besides, the microstructure and magnetic properties of these samples, and correlation between them will be revealed.

Keywords: M-type hexaferrite, substitution, cell parameter, magnetic properties

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Authors: Tatsuhiko Aizawa, Yohei Suzuki, Tomomi Shiratori

Abstract:

The austenitic stainless steel type AISI316 has been widely utilized as structural members and mold die substrates. The low temperature plasma nitriding has been utilized to harden these AISI316 members, parts, and dies without loss of intrinsic corrosion resistance to AISI316 stainless steels. Formation of CrN precipitates by normal plasma nitriding processes resulted in severe deterioration of corrosion toughness. Most previous studies on this low temperature nitriding of AISI316 only described the lattice expansion of original AISI316 lattices by the occupation of nitrogen interstitial solutes into octahedral vacancy sites, the significant hardening by nitrogen solid solution, and the enhancement of corrosion toughness. In addition to those engineering items, this low temperature nitriding process was characterized by the nitrogen supersaturation and nitrogen diffusion processes. The nitrogen supersaturated zones expanded by the nitrogen solute occupation to octahedral vacancy sites, and the un-nitrided surroundings to these zones were plastically strained to compensate for the mismatch strains across these nitrided and nitrided zones. The microstructure of nitrided AISI316 was refined by this plastic straining. The nitrogen diffusion process was enhanced to transport nitrogen solute atoms through the refined zone boundaries. This synergetic collaboration among the nitrogen supersaturation, the lattice expansion, the plastic straining, and the grain refinement yielded a thick nitrogen supersaturated layer. This synergetic relation was also characterized by the multilevel two-phase structuring. In XRD (X-Ray Diffraction) analysis, the nitrided AISI316 layer had - and -phases with the peak shifts from original lattices. After EBSD (Electron Back Scattering Diffraction) analysis, -grains and -grains homogeneously distributed in the nitrided layer. The scanning transmission electron microscopy (STEM) revealed that g-phase zone is N-poor cluster and a-phase zone is N-rich cluster. This proves that nitrogen supersaturated AISI316 stainless steels have multi-level two-phase structure in a very fine granular system.

Keywords: AISI316 stainless steels, chemical affinity to nitrogen solutes, multi-level two-phase structuring, nitrogen supersaturation

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Authors: Rizwan Ahmed Bhutto, Noor ul ain Hira Bhutto, Mingwei Wang, Shahid Iqbal, Jiang Yi

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Curcumin, a natural polyphenolic compound, boasts numerous health benefits; however, its industrial applications are hindered by instabilities and poor solubility. Encapsulating curcumin in Pickering emulsion presents a promising strategy to enhance its bioavailability. Yet, the development of an efficient and straightforward method to fabricate a natural emulsifier for Pickering emulsion poses a significant challenge. Chitosan has garnered attention due to its non-toxicity and excellent emulsifying properties. This study aimed to prepare four distinct types of self-aggregated chitosan particles using a pH-responsive self-assembling approach. The properties of the aggregated particles were adjusted by pH, degree of deacetylation (DDA), and molecular weight (MW), thereby controlling surface charge, size (ranging from nano to micro and floc), and contact angle. Pickering emulsions were then formulated using these various aggregated particles. As MW and pH increased and DDA decreased, the networked structures of the aggregated particles formed, resulting in highly elastic gels that were more resistant to the breakdown of Pickering emulsion at ambient temperature. With elevated temperatures, the kinetic energy of the aggregated particles increased, disrupting hydrogen bonds and potentially transforming the systems from fluids to gels. The Pickering emulsion based on aggregated particles served as a carrier for curcumin encapsulation. It was observed that DDA and MW played crucial roles in regulating drug loading, encapsulation efficiency, and release profile. This research sheds light on selecting suitable chitosan for controlling the release of bioactive compounds in Pickering emulsions, considering factors such as adjustable rheological properties, microstructure, and macrostructure. Furthermore, this study introduces an environmentally friendly and cost-effective synthesis of pH-responsive aggregate particles without the need for high-pressure homogenizers. It underscores the potential of aggregate particles with various MWs and DDAs for encapsulating other bioactive compounds, offering valuable applications in industries including food, flavor/fragrance, cosmetics, and medicine.

Keywords: chitosan, molecular weight, rheological properties, curcumin encapsulation

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