Search results for: microstructural characterization

Authors: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

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Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: ceramics, energy storage, electrochemical measurements, transmission electron microscope

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Authors: Luiz C. G. Pennafort Jr., Alexandre de S. Rios, Enio P. de Deus

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In the search for materials that replace conventional polymers in order to preserve natural resources, combined with the need to minimize the problems arising from environmental pollution generated by plastic waste, comes the recycled materials biodegradable, especially the composites reinforced with natural fibers. However, such materials exhibit properties little known, requiring studies of manufacturing methods and characterization of these composites. This article shows informations about preparation and characterization of a composite produced by extrusion, which consists of recycled PVC derived from the recycling of materials discarded, added of the micronized coconut fiber. The recycled PVC with 5% of micronized fiber were characterized by X-ray diffraction, thermogravimetric, differential scanning calorimetry, mechanical analysis and optical microscopy. The use of fiber in the composite caused a decrease in its specific weight, due to the lower specific weight of fibers and the appearance of porosity, in addition to the decrease of mechanical properties.

Keywords: recycled PVC, coconut fiber, characterization, composites

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Authors: S. Boudali, A. M. Soliman, B. Abdulsalam, K. Ayed, D. E. Kerdal, S. Poncet

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This study investigates the potential of using crushed concrete as aggregates to produce green and sustainable concrete. Crushed concrete was sieved to powder fine recycled aggregate (PFRA) less than 80 µm and coarse recycled aggregates (CRA). Physical, mechanical, and microstructural properties for PFRA and CRA were evaluated. The effect of the additional rates of PFRA and CRA on strength development of recycled aggregate concrete (RAC) was investigated. Additionally, the characteristics of interfacial transition zone (ITZ) between cement paste and recycled aggregate were also examined. Results show that concrete mixtures made with 100% of CRA and 40% PFRA exhibited similar performance to that of the control mixture prepared with 100% natural aggregate (NA) and 40% natural pozzolan (NP). Moreover, concrete mixture incorporating recycled aggregate exhibited a slightly higher later compressive strength than that of the concrete with NA. This was confirmed by the very dense microstructure for concrete mixture incorporating recycled concrete aggregates compared to that of conventional concrete mixture.

Keywords: compressive strength, recycled concrete aggregates, microstructure, interfacial transition zone, powder fine recycled aggregate

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Authors: Duygu Yüksel Deniz, Memet Vezir Kahraman, Serap Erdem Kuruca, Mediha Süleymanoğlu

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Our first aim was to synthesize Hydroxy Apatite (HAP) and then modify its surface by adding 4-Vinylbenzene boronic acid (4-VBBA). The characterization was done by FT-IR. By adding Polyvinyl alcohol (PVA) to 4- VBBA-HAP, we obtained a suitable electrospinning solution. PVA solution which was also modified by using alkoxy silanes, in order to prevent the scaffolds from being damaged by aqueous cell medium, was added. Keratin was dissolved and then added into the electrospinning solution. Keratin containing 4-VBBA- HAP/PVA composite was used to fabricate nanofiber scaffolds with the simultaneous UV-reactive electrospinning technique. The structural characterization was done by FT-IR. Thermal gravimetric analysis was also performed by using TGA. The morphological characterization was determined by SEM analyses. Our second aim was to create a scaffold where cells could grow. With this purpose, suitable nanofibers were choosen according to their SEM analysis. Keratin containing nanofibers were seeded with 3T3, ECV and SAOS cells and their cytotoxicity and cell proliferation were investigated by using MTT assay. After cell culturing process morphological characterization was determined by SEM analyses. These scaffolds were designed to be nontoxic biomaterials. Here, a comparision was made between keratin containing 3T3, ECV and SAOS seeded nanofiber scaffolds and the results were presented and discussed.

Keywords: cell culture, keratin, nanofibers, UV-reactive electrospinning

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Authors: H. A. Brandão Cordeiro, M. G. Bocardo, N. C. Penteado, V. T. de Moraes, S. M. Giampietri Lebrão, G. W. Lebrão

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The present study desired to obtain a nanocomposite of epoxy resin reinforced with graphene oxide (OG), for aerospace application, produced by aqueous emulsion. It was obtained proof bodies with 0.00 wt%, 0.10 wt%, 0.25 wt% and 0.50 wt% in weight of nanoparticles, to check the influence of it in the final quality of the obtained product. The validation of the results was done by the application thermal characterization by differential scanning calorimetry (DSC). It was seen that the nanocomposite reinforced with 0.10 wt% of OG showed the best results, the average glass transition temperature, at 2 °C, compared to the pure resin.

Keywords: aqueous emulsion, graphene, nanocomposites, thermal characterization

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Authors: Daniela Rivera-Tobar Mario Perez-Won, Roberto Lemus-Mondaca, Gipsy Tabilo-Munizaga

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Different dietary trends worldwide seek to consume foods with anti-inflammatory properties, rich in antioxidants, proteins, and unsaturated fatty acids that lead to better metabolic, intestinal, mental, and cardiac health. In this sense, food matrices with high protein content based on macro and microalgae are an excellent alternative to meet the new needs of consumers. An emerging and environmentally friendly technology for producing protein matrices is ultrasonic agglomeration. It consists of the formation of permanent bonds between particles, improving the agglomeration of the matrix compared to conventionally agglomerated products (compression). Among the advantages of this process are the reduction of nutrient loss and the avoidance of binding agents. The objective of this research was to optimize the ultrasonic agglomeration process in matrices composed of Spirulina (Arthrospira platensis) powder and Cochayuyo (Durvillae Antartica) flour, by means of the response variable (Young's modulus) and the independent variables were the process conditions (percentage of ultrasonic amplitude: 70, 80 and 90; ultrasonic agglomeration times and cycles: 20, 25 and 30 seconds, and 3, 4 and 5). It was evaluated using a central composite design and analyzed using response surface methodology. In addition, the effects of agglomeration on thermophysical and microstructural properties were evaluated. It was determined that ultrasonic compression with 80 and 90% amplitude caused conformational changes according to Fourier infrared spectroscopy (FTIR) analysis, the best condition with respect to observed microstructure images (SEM) and differential scanning calorimetry (DSC) analysis, was the condition of 90% amplitude 25 and 30 seconds with 3 and 4 cycles of ultrasound. In conclusion, the agglomerated matrices present good macro and microstructural properties which would allow the design of food systems with better nutritional and functional properties.

Keywords: ultrasonic agglomeration, physical properties of food, protein matrices, macro and microalgae

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Authors: Cise Unluer

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Reactive MgO hydrates to form brucite (Mg(OH)2, magnesium hydroxide), which can then react with CO2 and additional water to form a range of strength providing hydrated magnesium carbonates (HMCs) within cement-based formulations. The presented work focuses on the use of reactive MgO in a range of concrete mixes, where it carbonates by absorbing CO2 and gains strength accordingly. The main goal involves maximizing the amount of CO2 absorbed within construction products, thereby reducing the overall environmental impact of the designed formulations. Microstructural analyses including scanning electron microscopy (SEM), X-ray diffraction (XRD) and thermogravimetry/differential thermal analysis (TG/DTA) are used in addition to porosity, permeability and unconfined compressive strength (UCS) testing to understand the performance mechanisms. XRD Reference Intensity Ratio (RIR), acid digestion and TG/DTA are utilized to quantify the amount of CO2 sequestered, with the goal of achieving 100% carbonation through careful mix design, leading to a range of carbon neutral products with high strengths. As a result, samples stronger than those containing Portland cement (PC) were produced, revealing the link between the mechanical performance and microstructural development of the developed formulations with the amount of CO2 sequestered.

Keywords: carbonation, compressive strength, reactive MgO cement, sustainability

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Authors: Maryam Kiani

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The aim of this study was to investigate the influence of carbon black additive on the properties of fly ash-based geopolymer. The geopolymer samples were prepared using fly ash as the primary source material, along with an alkali activator solution and different concentrations of carbon black additive. The effects of carbon black on the geopolymer binder were evaluated by analyzing the compressive strength, flexural strength, water absorption, and microstructural properties of the cured samples. The results revealed that the inclusion of carbon black additive significantly enhanced the mechanical properties of the geopolymer binder. The compressive and flexural strengths were found to increase with the addition of carbon black, showing improvements of up to 25% and 15%, respectively. Moreover, the water absorption of the geopolymer samples reduced due to the presence of carbon black, indicating improved resistance against water permeability. Microstructural analysis using scanning electron microscopy (SEM) revealed a more compact and homogenous structure in the geopolymer samples with carbon black. The dispersion of carbon black particles within the geopolymer matrix was observed, suggesting improved interparticle bonding and increased densification. Overall, this study demonstrates the positive impact of carbon black additive on the qualities of fly ash-based geopolymer, emphasizing its potential as an effective enhancer for geopolymer binder applications.

Keywords: fly-ash, carbon black, nanotechnology, geopolymer

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Authors: F. Villaret, I. Jacot, Y. Shen, Z. Kong, T. XU, Y. Wang, D. Lu

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Wire Arc Additive Manufacturing (WAAM) allows the rapid production of large, homogeneous parts with complex geometry. However, in the nuclear field, parts can reach dimensions of ten to a hundred tons. In this case, the usual WAAM TIG or CMT processes do not have sufficient deposition rates to consider the manufacture of parts of such dimensions within a reasonable time. The submerged arc welding process (SAW, Submerged Arc Welding) allows much higher deposition rates. Although there are very few references to this process for additive manufacturing in the literature, it has been used for a long time for the welding and coating of nuclear power plant vessels, so this process is well-known and mastered as a welding process. This study proposes to evaluate the SAW process as an additive manufacturing technique by taking as an example a low-alloy steel of type 16MND5. In the first step, a parametric study allowed the evaluation of the effect of the different parameters and the deposition rate on the geometry of the beads and their microstructure. Larger parts were also fabricated and characterized by metallography and mechanical tests (tensile, impact, toughness). The effect of different heat treatments on the microstructure is also studied.

Keywords: WAAM, low alloy steel, submerged arc, caracterization

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Authors: Wenjin Zhu, Ian E. Jacobs, Henning Sirringhaus

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We have demonstrated a model system for the controlled incorporation of tie-chains into semicrystalline conjugated polymers using blends of different molecular weights that leads to a significant increase in electrical conductivity. Through careful assessment of the microstructural evolution upon tie chain incorporation we have demonstrated that no major changes in phase morphology or structural order in the crystalline domains occur and that the observed enhancement in electrical conductivity can only be explained consistently by tie chains facilitating the transport across grain boundaries between the crystalline domains. Here we studied the thermoelectric properties of aligned, ion exchange-doped ribbon phase PBTTT with blends of different molecular weight components. We demonstrate that in blended films higher electrical conductivities (up to 4810.1 S/cm), Seebeck coefficients and thermoelectric power factors of up to 172.6 μW m-1 K-2 can be achieved than in films with single component molecular weights. We investigate the underpinning thermoelectric transport physics, including structural and spectroscopic characterization, to better understand how controlled tie chain incorporation can be used to enhance the thermoelectric performance of aligned conjugated polymers.

Keywords: organic electronics, thermoelectrics, conjugated polymers, tie chain

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Authors: Carlos Caro, Ernest Blade, Nestor Rojas

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This study determined the relationship between basic geo-technical parameters and parameters of the hydro logical model Thomas for water balance of rural watersheds, as a methodological calibration application, applicable in distributed models as IBER model, which represents a distributed system simulation models for unsteady flow numerical free surface. There was an exploration in 25 points (on 15 sub) basin of Rio Piedras (Boy.) obtaining soil samples, to which geo-technical characterization was performed by laboratory tests. Thomas model has a physical characterization of the input area by only four parameters (a, b, c, d). Achieve measurable relationship between geo technical parameters and 4 values of hydro logical parameters helps to determine subsurface, underground and surface flow more agile manner. It is intended in this way to reach some solutions regarding limits initial model parameters on the basis of Thomas geo-technical characterization. In hydro geological models of rural watersheds, calibration is an important process in the characterization of the study area. This step can require a significant computational cost and time, especially if the initial values or parameters before calibration are outside of the geo-technical reality. A better approach in these initial values means optimization of these process through a geo-technical materials area, where is obtained an important approach to the study as in the starting range of variation for the calibration parameters.

Keywords: distributed hydrology, hydrological and geotechnical characterization, Iber model

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Authors: H. Özkan Gülsoy, Antonyraj Arockiasamy

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The application of powder injection molding technology for the fabrication of metallic and non-metallic components is of growing interest as the process considerably saves time and cost. Utilizing this fabrication method, full dense components are being prepared in various sizes. In this work, our effort is focused to study the densification behavior of the parts made using different size 316L stainless steel powders. The metal powders were admixed with an adequate amount of polymeric compounds and molded as standard tensile bars. Solvent and thermal debinding was carried out followed by sintering in ultra pure hydrogen atmosphere based on the differential scanning calorimetry (DSC) cycle. Mechanical property evaluation and microstructural characterization of the sintered specimens was performed using universal Instron tensile testing machine, Vicker’s microhardness tester, optical (OM) and scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction were used. The results are compared and analyzed to predict the strength and weakness of the test conditions.

Keywords: powder injection molding, sintering, particle size, stainless steels

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Authors: Renu Kumari, Jyotsna Dutta Majumdar

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In the present study, composite coating consisting of hydroxyapatite (HA) + 50 wt% TiO2 has been developed on Ti-6Al-4V substrate by plasma spray deposition technique. Followed by plasma spray deposition, detailed surface roughness and microstructural characterization were carried out by using optical profilometer and scanning electron microscopy (SEM), respectively. The composition and phase analysis were carried out by energy-dispersive X-ray spectroscopy analysis, and X-ray diffraction (XRD) technique, respectively. The bio-activity behavior of the uncoated and coated samples was also compared by dipping test in Hank’s solution. The average surface roughness of the coating was 10 µm (as compared to 0.5 µm of as-received Ti-6Al-4V substrate) with the presence of porosities. The microstructure of the coating was found to be continuous with the presence of solidified splats. A detailed XRD analysis shows phase transformation of TiO2 from anatase to rutile, decomposition of hydroxyapatite, and formation of CaTiO3 phase. Standard dipping test confirmed a faster kinetics of deposition of calcium phosphate in the coated HA+50% wt.% TiO2 surface as compared to the as-received substrate.

Keywords: titanium, plasma spraying, microstructure, bio-activity, TiO2, hydroxyapatite

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Authors: H. Gonzalez-Rivera, J. L. Palmeros-Torres

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This paper describes the application of traditional computer vision techniques as a procedure for automatic measurement of the secondary dendrite arm spacing (SDAS) from microscopic images. The algorithm is capable of finding the lineal or curve-shaped secondary column of the main microstructure, measuring its length size in a micro-meter and counting the number of spaces between dendrites. The automatic characterization was compared with a set of 1728 manually characterized images, leading to an accuracy of −0.27 µm for the length size determination and a precision of ± 2.78 counts for dendrite spacing counting, also reducing the characterization time from 7 hours to 2 minutes.

Keywords: dendrite arm spacing, microstructure inspection, pattern recognition, polynomial regression

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Authors: Maria Santana, Jose Estaire

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Even though recycling strategies are becoming more important in recent years, there is still a huge amount of industrial by-products that are the disposal of at landfills. Due to the size, possible dangerous composition, and heterogeneity, most of the wastes are located at landfills without a basic geotechnical characterization. This lack of information may have an important influence on the correct stability calculations. This paper presents the results of geotechnical characterization of some industrial wastes disposed at one landfill. The shear strength parameters were calculated based on direct shear test results carried out in a large shear box owned by CEDEX, which has a shear plane of 1 x 1 m. These parameters were also compared with the results obtained in a 30 x 30 cm shear box. The paper includes a sensitive analysis of the global safety factor of the landfill's overall stability as a function of shear strength variation. The stability calculations were assessed for various hydrological scenarios to simulate the design and performance of the leachate drainage system. The characterization was completed with leachate tests to study the potential impact on the environment.

Keywords: industrial wastes, landfill, leachate tests, stability

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Authors: D. Falliano, D. De Domenico, G. Ricciardi, E. Gugliandolo

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This paper is focused on the mechanical characterization of foamed concrete specimens with protein-based foaming agent. Unlike classic foamed concrete, a peculiar property of the analyzed foamed concrete is the extrudability, which is achieved via a specific additive in the concrete mix that significantly improves the cohesion and viscosity of the fresh cementitious paste. A broad experimental campaign was conducted to evaluate the compressive strength and the indirect tensile strength of the specimens. The study has comprised three different cement types, two water/cement ratios, three curing conditions and three target dry densities. The variability of the strength values upon the above mentioned factors is discussed.

Keywords: cement type, curing conditions, density, extrudable concrete, foamed concrete, mechanical characterization

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Authors: Francisco J. Ortega, Claudia Roman, Moisés García-Morales, Francisco J. Navarro

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Asphaltic bitumen has been largely used in both industrial and civil engineering, mostly in pavement construction and roofing membrane manufacture. However, bitumen as such is greatly susceptible to temperature variations, and dramatically changes its in-service behavior from a viscoelastic liquid, at medium-high temperatures, to a brittle solid at low temperatures. Bitumen modification prevents these problems and imparts improved performance. Isocyanates like polymeric MDI (mixture of 4,4′-diphenylmethane di-isocyanate, 2,4’ and 2,2’ isomers, and higher homologues) have shown to remarkably enhance bitumen properties at the highest in-service temperatures expected. This comes from the reaction between the –NCO pendant groups of the oligomer and the most polar groups of asphaltenes and resins in bitumen. In addition, oxygen diffusion and/or UV radiation may provoke bitumen hardening and ageing. With the purpose of minimizing these effects, nano-layered-silicates (nanoclays) are increasingly being added to bitumen formulations. Montmorillonites, a type of naturally occurring mineral, may produce a nanometer scale dispersion which improves bitumen thermal, mechanical and barrier properties. In order to increase their lipophilicity, these nanoclays are normally treated so that organic cations substitute the inorganic cations located in their intergallery spacing. In the present work, the combined effect of polymeric MDI and the commercial montmorillonite Cloisite® 20A was evaluated. A selected bitumen with penetration within the range 160/220 was modified with 10 wt.% Cloisite® 20A and 2 wt.% polymeric MDI, and the resulting ternary composites were characterized by linear rheology, X-ray diffraction (XRD) and Atomic Force Microscopy (AFM). The rheological tests evidenced a notable solid-like behavior at the highest temperatures studied when bitumen was just loaded with 10 wt.% Cloisite® 20A and high-shear blended for 20 minutes. However, if polymeric MDI was involved, the sequence of addition exerted a decisive control on the linear rheology of the final ternary composites. Hence, in bitumen/Cloisite® 20A/polymeric MDI formulations, the previous solid-like behavior disappeared. By contrast, an inversion in the order of addition (bitumen/polymeric MDI/ Cloisite® 20A) enhanced further the solid-like behavior imparted by the nanoclay. In order to gain a better understanding of the factors that govern the linear rheology of these ternary composites, a morphological and microstructural characterization based on XRD and AFM was conducted. XRD demonstrated the existence of clay stacks intercalated by bitumen molecules to some degree. However, the XRD technique cannot provide detailed information on the extent of nanoclay delamination, unless the entire fraction has effectively been fully delaminated (situation in which no peak is observed). Furthermore, XRD was unable to provide precise knowledge neither about the spatial distribution of the intercalated/exfoliated platelets nor about the presence of other structures at larger length scales. In contrast, AFM proved its power at providing conclusive information on the morphology of the composites at the nanometer scale and at revealing the structural modification that yielded the rheological properties observed. It was concluded that high-shear blending brought about a nanoclay-reinforced network. As for the bitumen/Cloisite® 20A/polymeric MDI formulations, the solid-like behavior was destroyed as a result of the agglomeration of the nanoclay platelets promoted by chemical reactions.

Keywords: Atomic Force Microscopy, bitumen, composite, isocyanate, montmorillonite.

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Authors: Dong Zhang, Kang Hai Tan, Aravind Dasari

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Increasing concern on environmental sustainability and waste management has driven the construction and building sector towards renewable materials. In this work, we have explored the usage of natural fibers as an alternative to synthetic fibers like polypropylene (PP) in ultra-high performance concrete (UHPC). PP fibers are incorporated into concrete to resist explosive thermal spalling of UHPC during a fire exposure scenario. Experimental studies on the effect of natural fiber on the mechanical properties and spalling resistance of UHCP were conducted. The residual mechanical properties of UHPC with natural fibers were tested after heating to different temperatures. Spalling behavior of UHPC with natural fibers is also assessed by heating the samples according to ISO 834 fire curve. A range of analytical, physical and microscopic characterization techniques was also used on the concrete samples before and after being subjected to elevated temperature to investigate the phase and microstructural change of the sample. The findings show that natural fibers are able to improve fire resistance of UHPC. Adding natural fibers can prevent UHPC from spalling at high temperature. This study provides an alternative, which is at low cost and environmentally friendly, to prevent spalling of UHPC.

Keywords: high temperature, natural fiber, spalling, ultra-high performance concrete

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Authors: Med. A. Djeridane, M. Ferhat, H. A. Benhorma, O. Bouledroua

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This research is dedicated to exploring the failure of a turbine blade within a gas transportation plant, with a primary focus on conducting a comprehensive examination through advanced metallurgical and mechanical analyses of the identified failed blade. Crafted from the nickel superalloy Inconel IN738LC, the turbine engine had accumulated approximately 61,000 operational hours before the blades failed, causing severe damage to the transportation plant and necessitating a prolonged shutdown. The investigative procedure commenced with an in-depth visual inspection of the blade surfaces, succeeded by fractography analysis of the fracture surfaces, microstructural investigations, chemical analysis, and hardness measurements. The findings unveiled distinctive fatigue marks on the fracture surface. Critical microstructural changes were identified as a consequence of the blade's operation at high temperatures. The investigation determined that the crack initiation resulted from coating damage at the leading edge, subsequently propagating through fatigue. Ultimately, due to a reduction in cross-sectional area, the fracture was completed. This comprehensive analysis sheds light on the intricate factors contributing to turbine blade failure and offers valuable insights for enhancing operational reliability in similar environments.

Keywords: gas turbine, blade failure, TCP phases, fatigue, quantitative analysis

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Authors: Gerrit Ter Haar, Thorsten Becker, Deborah Blaine

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The Additive Manufacturing (AM) process of Selective Laser Melting (SLM) has seen an exponential growth in sales and development in the past fifteen years. Whereas the capability of SLM was initially limited to rapid prototyping, progress in research and development (R&D) has allowed SLM to be capable of fully functional parts. This technology is still at a primitive stage and technical knowledge of the vast number of variables influencing final part quality is limited. Ongoing research and development of the sensitive printing process and post processes is of utmost importance in order to qualify SLM parts to meet international standards. Quality concerns in Ti-6Al-4V manufactured through SLM has been identified, which include: high residual stresses, part porosity, low ductility and anisotropic mechanical properties. Whereas significant quality improvements have been made through optimising printing parameters, research indicates as-produced part ductility to be a major limiting factor when compared to its wrought counterpart. This study aims at achieving an in-depth understanding of the underlining links between SLM produced Ti-6Al-4V microstructure and its mechanical properties. Knowledge of microstructural transformation kinetics of Ti-6Al-4V allows for the optimisation of post-process heat treatments thereby achieving the required process route to manufacture high quality SLM produced Ti-6Al-4V parts. Experimental methods used to evaluate the kinematics of microstructural transformation of SLM Ti-6Al-4V are: optical microscopy and electron backscatter diffraction. Results show that a low-temperature heat treatment is capable of transforming the as-produced, martensitic microstructure into a duel-phase microstructure exhibiting both a high strength and improved ductility. Furthermore, isotropy of mechanical properties can be achieved through certain annealing routes. Mechanical properties identical to that of wrought Ti-6Al-4V can, therefore, be achieved through an optimised process route.

Keywords: EBSD analysis, heat treatments, microstructural characterisation, selective laser melting, tensile behaviour, Ti-6Al-4V

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Authors: Mitsuhiro Okayasu, Lele Yang, Koji Shimotsu

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The effects of microstructural characteristics on the mechanical and hydrogen embrittlement properties of 1,800MPa grade hot stamping carbon steel were investigated experimentally. The tensile strength increased with increasing the hot stamping temperature until around 921°C, but that decreased with increasing the temperature in more than 921°C due to the increment of the size of lath martensite and prior austenite. With the hot stamping process, internal strain was slightly created in the sample, which led to the slight increment of the hardness value although no clear change of the microstructural formation was detected. Severity of hydrogen embrittlement was investigated using the hot stamped carbon steels after the immersion in a hydrogen gas, and that was directly attributed to the infiltration of the hydrogen into their grain boundaries. The high strength carbon steel with tiny lath martensite microstructure could make severe hydrogen brittleness as the hydrogen was strongly penetrated in the grain boundaries in the hydrogen gas for a month. Because of weak embrittlement for the as-received carbon (ferrite and pearlite), hydrogen embrittlement is caused by the high internal strain and high dislocation density. The hydrogen embrittlement for carbon steel is attributed to amount of the hydrogen immersed in-between grain boundaries, which is caused by the dislocation density and internal strain.

Keywords: hydrogen embrittlement, hot stamping process, carbon steel, mechanical property

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Authors: Mohammad Khattak, Bikash Adhikari, Sambodh Adhikari

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This research deals with the physical, microstructural, mechanical, and shrinkage characteristics of flyash-based soil-geopolymer mixtures. Medium and high plastic soils were obtained from local construction projects. Class F flyash was used with a mixture of sodium silicate and sodium hydroxide solution to develop soil-geopolymer mixtures. Several mixtures were compacted, cured at different curing conditions, and tested for unconfined compressive strength (UCS), linear shrinkage, and observed under scanning electron microscopy (SEM). The results of the study demonstrated that the soil-geopolymer mixtures fulfilled the UCS criteria of cement treated design (CTD) and cement stabilized design (CSD) as recommended by the department of transportation for pavement base and subbase layers. It was found that soil-geopolymer demonstrated either similar or better UCS and shrinkage characteristics relative to conventional soil-cement mixtures. The SEM analysis revealed that microstructure of soil-geopolymer mixtures exhibited development and steady growth of geopolymerization during the curing period. Based on mechanical, shrinkage, and microstructural characteristics it was suggested that the soil-geopolymer mixtures, has an immense potential to be used as pavement subgrade, subbase, and base layers.

Keywords: soil-geopolymer, pavement base, soil stabilization, unconfined compressive strength, shrinkage, microstructure, and morphology

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Authors: Nithin Krisshna Gunasekaran, Prathima Prabhu Tumkur, Nicole Nazario Bayon, Krishnan Prabhakaran, Joseph C. Hall, Govindarajan T. Ramesh

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Cerium oxide and turmeric have antioxidant properties, which have gained interest among researchers to study their applications in the field of biomedicine, such asanti-inflammatory, anticancer, and antimicrobial applications. In this study, the turmeric extract was prepared and mixed with cerium nitrate hexahydrate, stirred continuously to obtain a homogeneous solution and then heated on a hot plate to get the supernatant evaporated, then calcinated at 600°C to obtain the cerium oxide nanoparticles. Characterization of synthesized cerium oxide nanoparticles through Scanning Electron Microscopy determined the particle size to be in the range of 70 nm to 250 nm. Energy Dispersive X-Ray Spectroscopy determined the elemental composition of cerium and oxygen. Individual particles were identified through the characterization of cerium oxide nanoparticles using Field Emission Scanning Electron Microscopy, in which the particles were determined to be spherical and in the size of around 70 nm. The presence of cerium oxide was assured by analyzing the spectrum obtained through the characterization of cerium oxide nanoparticles by Fourier Transform Infrared Spectroscopy. The crystal structure of cerium oxide nanoparticles was determined to be face-centered cubic by analyzing the peaks obtained through theX-Ray Diffraction method. The crystal size of cerium oxide nanoparticles was determined to be around 13 nm by using the Debye Scherer equation. This study confirmed the synthesis of cerium oxide nanoparticles using turmeric extract.

Keywords: antioxidant, characterization, cerium oxide, synthesis, turmeric

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Authors: M. Ravindiran, P. Shankar

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This paper deals with the comparison of two synthesis methods, namely, sol-gel, and combustion to prepare Fe doped ZnO nano material. Characterization results for structural, optical and magnetic properties were analyzed for the sol gel and combustion synthesis derived materials. Magnetic studies of the prepared compounds reveal that the combustion synthesis derived material has good magnetization of 50 emu/gm with a better hysteresis loop curve.

Keywords: DMS, combustion, ferromagnetic, synthesis methods

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Authors: F. Z. Benabid, S. Kridi, F. Zouai, D. Benachour

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The aim of present work is to characterize the PVDF/TiO2 blends as nanocomposites, and study the effect of TiO2 on properties of different compositions and the evaluation of the effectiveness of the method used for filler treatment. Nanocomposite samples were synthesized by molten route in an internal mixer. The TiO2 nanoparticles were treated with stearic acid in order to obtain a good dispersion, and the demonstration of the effectiveness of the treatment on the morphology and roughness of the nanofiller was established by microstructural analysis by FTIR and AFM. The various developed nanocomposite compositions were characterized by different methods; i.e. FTIR, XRD, SEM and optical microscopy. Rheological, dielectric and mechanical studies were also performed. The results showed a remarkable increase in the crystallinity of the PVDF/neat TiO2 nanocomposite containing 1 wt% loading of filler, due to the nucleation effect of TiO2 nanoparticles. A good dispersion was obtained in PVDF/treated TiO2 nanocomposites. The rheological study showed an increase in the fluidity in all developed nanocomposite compositions, involved by the orientation of TiO2 nanoparticles in the flow direction. The dielectric study revealed an increase in electrical conductivity in PVDF/neat TiO2 nanocomposites. However, in PVDF/ treated TiO2 nanocomposites, the electrical conductivity was decreased by the addition of 0.5 and 2 wt% loading of filler.

Keywords: nanocomposites, PVDF, TiO2, comixing, mechanical treatment

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Authors: Mitia Ramarosaona, Sylvie Castagnet, Damien Halm, Henri-Alexandre Cayzac, Nicolas Dufaure, Philippe Papin

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In light of the ongoing energy transition, 'Infrastructure developments' for hydrogen transportation and storage raise studies on the materials employed for hyperbaric vessels. Type IV tanks represent the most mature choice for gaseous hydrogen storage at high pressure – 70MPa. These tanks are made of a composite shell and an internal hydrogen-exposed polymer liner. High pressure conditions lead to severe mechanical loading requiring high resistance. Liner is in contact with hydrogen and undergoes compression – decompression cycles during system filling and emptying. Stresses induced by this loading, coupled with hydrogen diffusion, were found to cause microstructural changes and degradation of mechanical behaviour after decompression phase in some studies on HDPE. These phenomena are similar to those observed in elastomeric components like sealing rings, which can affect permeability and lead to their failure. They may lead to a hydrogen leak, compromising security and tightness of the tank. While these phenomena have been identified in elastomers, they remain less addressed in thermoplastics and consequences post-decompression damages on mechanical behaviour and to the best of author's knowledge was not studied either. Different additives are also included in liner formulation to improve its behaviour. This study aimed to better understand damage micro-mechanisms in PA11s exposed to hydrogen compression-decompression cycles and understand if additives influence their resistance. Samples of pure, plasticized and impact-modified PA11s are exposed to 1, 3 and 8 pressure cycles including hydrogen saturation at 70MPa followed by severe 15-second decompression. After hydrogen exposure and significantly later than full desorption, the residual mechanical behaviour is characterized through impact and monotonic tensile tests, on plain and notched samples. Several techniques of microstructure and micro-nano damage characterization are carried out to assess whether changes in macroscopic properties are driven by microstructural changes in the crystalline structure (SAXS-WAXS acquisitions and SEM micrographs). Thanks to WAXS acquisition and microscopic observation, the effects due to additives and pressure consequences can be decorrelated. Pure PA11 and PA11 with a low percentage of additives show an increase in stress level at the first yielding point after hydrogen cycles. The amplitude of the stress increase is more important in formulation with additives because of changes in PA11 matrix behavior and environment created by additives actions. Plasticizer modifies chain mobility leading to microstructure changes while other additives, more ductile than PA11, is able to cavitate inside PA11 matrix when undergoing decompression. On plasticized formulation, plasticizer migration are suspected to enhance impact of hydrogen cycling on mechanical behaviour. Compared to the literature on HDPE and elastomers, no damages like cavitation or cracking could be evidenced from SAXS experiments on every PA11 formulation tested. In perspectives, on all formulation, experimental work is underway to confirm influence of residual pressure level after decompression on post-decompression damages level, the aim is to better understand the factors affecting the mechanical behavior of thermoplastics subject to mechanical solicitation from decompression in hydrogen tank liners, not mechanical behaviour of liner in hydrogen tanks directly.

Keywords: additives, hydrogen tank liner, microstructural analysis, PA11

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Authors: M. P. E. E Silva, A. M. Galloway, A. I. Toumpis

Abstract:

An increasing concern exists in the welding industry in terms of faster joining processes. Methods such as the alternation between shielding gases such Ar, CO₂ and He have been able to provide improved penetration of the joint, reduced heat transfer to the workpiece, and increased travel speeds of the welding torch. Nitrogen as a shielding gas is not desirable due to its reactive behavior within the arc plasma, being absorbed by the molten pool during the welding process. Below certain amounts, nitrogen is not harmful. However, the nitrogen threshold is reduced during the solidification of the joint, and if its subsequent desorption is not completed on time, gas entrapment and blowhole formation may occur. The present study expanded the use of the alternating shielding gas method in the gas metal arc welding (GMAW) process by alternately supplying Ar/5%N₂ and He. Improvements were introduced in terms of joint strength and grain refinement. Microstructural characterization findings showed porosity-free welds with reduced inclusion formation while mechanical tests such as tensile and bend tests confirmed the reinforcement of the joint by the addition of nitrogen. Additionally, significant reductions of the final distortion of the workpiece were found after the welding procedure as well as decreased heat affected zones and temperatures of the weld.

Keywords: alternating shielding gas method, GMAW, grain refinement, nitrogen, porosity, mechanical testing

Procedia PDF Downloads 106

Authors: Ahmad El Hajjar, Joanna Eid, Salima Bouchemella, Tariq Ouahbi, Benoit Duchemin, Said Taibi

Abstract:

In our present society, raw earth presents an alternative as an energy-saving building material for dealing with climate and environmental issues. Nevertheless, it has a sensitivity to water, due to the presence of fines, which has a direct effect on its consistency. This can be expressed during desiccation, by shrinkage deformations resulting in cracking that begins once the internal tensile stresses developed, due to suction, exceed the tensile strength of the material. This work deals with the evolution of the strain of clay samples, from the beginning of shrinkage until the initiation of crack, using the DIC (Digital Image Correlation) technique. In order to understand the origin of cracking, desiccation is studied for different boundary conditions and depending on the intrinsic characteristics of the material. On the other hand, a study of restrained shrinkage is carried out on the ring test to investigate the ultimate tensile strength from which the crack begins in the dough of clay. The purpose of this test is to find the type of reinforcement adapted to thwart in the cracking of the material. A microscopic analysis of the damaged area is necessary to link the macroscopic mechanisms of cracking to the various physicochemical phenomena at the microscopic scale in order to understand the different microstructural mechanisms and their impact on the macroscopic shrinkage.

Keywords: clayey soil, shrinkage, strain, cracking, digital image correlation

Procedia PDF Downloads 156

Authors: A. P. Srivastava, D. Srivastava, D. J. Browne

Abstract:

Relaxation dynamics of Zr44Cu40Al8Ag8 bulk metallic glass (BMG) has been probed using dynamic mechanical analyzer. The BMG sample was casted in the form of a plate of dimension 55 mm x 40 mm x 3 mm using tilt casting technique. X-ray diffraction and transmission electron microscope have been used for the microstructural characterization of as-cast BMG. For the mechanical spectroscopy study, samples in the form of a bar of size 55 mm X 2 mm X 3 mm were machined from the BMG plate. The mechanical spectroscopy was performed on dynamic mechanical analyzer (DMA) by 50 mm 3-point bending method in a nitrogen atmosphere. It was observed that two glass transition process were competing in supercooled liquid region around temperature 390°C and 430°C. The supercooled liquid state was completely characterized using DMA and differential scanning calorimeter (DSC). In addition to the main α-relaxation process, presence of β relaxation process around temperature 360°C; below the glass transition temperature was also observed. The β relaxation process could be described by Arrhenius law with the activation energy of 160 kJ/mole. The volume of the flow unit associated with this relaxation process has been estimated. The results from DMA study has been used to characterize the shear transformation zone in terms of activation volume and size. High fragility parameter value of 34 and higher activation volume indicates that this alloy could show good plasticity in supercooled liquid region. The possible mechanism for the relaxation processes has been discussed.

Keywords: DMA, glass transition, metallic glass, thermoplastic forming

Procedia PDF Downloads 290

Authors: Woei-Shyan Lee, Yu-Liang Chuang

Abstract:

The nano-mechanical properties of as-deposited Cu/Si thin films indented to a depth of 2000 nm are investigated using a nanoindentation technique. The nanoindented specimens are annealed at a temperature of either 160 °C or 210°C, respectively. The microstructures of the as-deposited and annealed samples are then examined via transmission electron microscopy (TEM). The results show that both the loading and the unloading regions of the load-displacement curve are smooth and continuous, which suggests that no debonding or cracking occurs during nanoindentation. In addition, the hardness and Young’s modulus of the Cu/Si thin films are found to vary with the nanoindentation depth, and have maximum values of 2.8 GPa and 143 GPa, respectively, at the maximum indentation depth of 2000 nm. The TEM observations show that the region of the Cu/Si film beneath the indenter undergoes a phase transformation during the indentation process. In the case of the as-deposited specimens, the indentation pressure induces a completely amorphous phase within the indentation zone. For the specimens annealed at a temperature of 160°C, the amorphous nature of the microstructure within the indented zone is maintained. However, for the specimens annealed at a higher temperature of 210°C, the indentation affected zone consists of a mixture of amorphous phase and nanocrystalline phase. Copper silicide (η-Cu3Si) precipitates are observed in all of the annealed specimens. The density of the η-Cu3Si precipitates is found to increase with an increasing annealing temperature.

Keywords: nanoindentation, Cu/Si thin films, microstructural evolution, annealing temperature

Procedia PDF Downloads 384