Search results for: austenitic microstructure

Authors: Andrea Cretu, Calin Cadar, Maria Miclaus, Lucian Barbu-Tudoran, Siegfried Stapf, Ioan Ardelean

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Additives and mineral admixtures have become an integral part of cement-based materials. It is common practice to add silica fume to cement based mixes in order to produce high-performance concrete. There is still a lack of scientific understanding regarding the effects that silica fume has on the microstructure of hydrated cement paste. The aim of the current study is to develop high-performance materials with low permeability and high resistance to flexural stress using silica fume and an organosilane. Organosilane bonds with cement grains and silica fume, influencing both the workability and the final properties of the mix, especially the pore size distributions and pore connectivity. Silica fume is a known pozzolanic agent which reacts with the calcium hydroxide in hydrated cement paste, producing more C-S-H and improving the mechanical properties of the mix. It is believed that particles of silica fume act as capillary pore fillers and nucleation centers for C-S-H and other hydration products. In order to be able to design cement-based materials with added silica fume and organosilane, it is necessary first to understand the formation of the porous network during hydration and to observe the distribution of pores and their connectivity. Nuclear magnetic resonance (NMR) methods in low-fields are non-destructive and allow the study of cement-based materials from the standpoint of their porous structure. Other methods, such as XRD and SEM-EDS, help create a comprehensive picture of the samples, along with the classic mechanical tests (compressive and flexural strength measurements). The transverse relaxation time (T₂) was measured during the hydration of 16 samples prepared with two water/cement ratios (0.3 and 0.4) and different concentrations or organosilane (APTES, up to 2% by mass of cement) and silica fume (up to 6%). After their hydration, the pore size distribution was assessed using the same NMR approach on the samples filled with cyclohexane. The SEM-EDS and XRD measurements were applied on pieces and powders prepared from the samples that were used in mechanical testing, which were kept under water for 28 days. Adding silica fume does not influence the hydration dynamics of cement paste, while the addition of organosilane extends the dormancy stage up to 10 hours. The size distribution of the capillary pores is not influenced by the addition of silica fume or organosilane, while the connectivity of capillary pores is decreased only when there is organosilane in the mix. No filling effect is observed even at the highest concentration of silica fume. There is an apparent increase in flexural strength of samples prepared only with silica fume and a decrease for those prepared with organosilane, with a few exceptions. XRD reveals that the pozzolanic reactivity of silica fume can only be observed when there is no organosilane present and the SEM-EDS method reveals the pore distribution, as well as hydration products and the presence or absence of calcium hydroxide. The current work was funded by the Romanian National Authority for Scientific Research, CNCS – UEFISCDI, through project PN-III-P2-2.1-PED-2016-0719.

Keywords: cement hydration, concrete admixtures, NMR, organosilane, porosity, silica fume

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Authors: Nilufar Chowdhury, Fereydoun Najafian Jazi, Omid Ghasemi-Fare

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The thermal effect on soil properties induces significant variations in hydraulic conductivity, which is attributable to temperature-dependent transitions in soil properties. With the elevation of temperature, there can be a notable increase in intrinsic permeability due to the degeneration of bound water molecules into a free state facilitated by thermal energy input. Conversely, thermal consolidation may cause a reduction in intrinsic permeability as soil particles undergo densification. This thermal response of soil permeability exhibits pronounced heterogeneity across different soil types. Furthermore, this temperature-induced disruption of the bound water within clay matrices can enhance the mineral-to-mineral contact, initiating irreversible deformation within the clay structure. This indicates that when soil undergoes heating-cooling cycles, plastic strain can develop, which needs to be investigated for every soil type to understand the thermo-hydro mechanical behavior of clay properly. This research aims to study the effect of the heating-cooling cycle on the intrinsic permeability and time-dependent evaluation of thermal volume change of sodium Bentonite clay. A temperature-controlled triaxial permeameter cell is used in this study. The selected temperature is 20° C, 40° C, 40° C and 80° C. The hydraulic conductivity of Bentonite clay under 100 kPa confining stresses was measured. Hydraulic conductivity analysis was performed on a saturated sample for a void ratio e = 0.9, corresponding to a dry density of 1.2 Mg/m3. Different hydraulic gradients were applied between the top and bottom of the sample to obtain a measurable flow through the sample. The hydraulic gradient used for the experiment was 4000. The diameter and thickness of the sample are 101. 6 mm, and 25.4 mm, respectively. Both for heating and cooling, the hydraulic conductivity at each temperature is measured after the flow reaches the steady state condition to make sure the volume change due to thermal loading is stabilized. Thus, soil specimens were kept at a constant temperature during both the heating and cooling phases for at least 10-18 days to facilitate the equilibration of hydraulic transients. To assess the influence of temperature-induced volume changes of Bentonite clay, the evaluation of void ratio change during this time period has been monitored. It is observed that the intrinsic permeability increases by 30-40% during the heating cycle. The permeability during the cooling cycle is 10-12% lower compared to the permeability observed during the heating cycle at a particular temperature. This reduction in permeability implies a change in soil fabric due to the thermal effect. An initial increase followed by a rapid decrease in void ratio was observed, representing the occurrence of possible osmotic swelling phenomena followed by thermal consolidation. It has been observed that after a complete heating-cooling cycle, there is a significant change in the void ratio compared to the initial void ratio of the sample. The results obtained suggest that Bentonite clay’s microstructure can change subject to a complete heating-cooling process, which regulates macro behavior such as the permeability of Bentonite clay.

Keywords: bentonite, permeability, temperature, thermal volume change

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Authors: Dhanesh Sing Das, Bharat Tadikonda Venkata

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Collapsible soils undergo significant volume reduction upon wetting under the pre-existing mechanically applied normal stress (inundation pressure). These soils exhibit a very high strength in air-dried conditions and can carry up to a considerable magnitude of normal stress without undergoing significant volume change. The soil strength is, however, lost upon saturation and results in a sudden collapse of the soil structure under the existing mechanical stress condition. The intrusion of water into the dry deposits of such soil causes ground subsidence leading to damages in the overlying buildings/structures. A study on the wetting-induced volume change behavior of collapsible soils is essential in dealing with the ground subsidence problems in various geotechnical engineering practices. The collapse of loosely compacted Kaolin soil upon wetting under various inundation pressures has been reported in recent studies. The collapse in the Kaolin soil is attributed to the alteration in the soil particle-particle association (fabric) resulting due to the changes in the various inter-particle (microscale) forces induced by the water saturation. The inundation pressure plays a significant role in the fabric evolution during the wetting process, thus controls the collapse potential of the compacted soil. A microstructural study is useful to understand the collapse mechanisms at various pore-fabric levels under different inundation pressure. Kaolin soil compacted to a dry density of 1.25 g/cc was used in this work to study the wetting-induced volume change behavior under different inundation pressures in the range of 10-1600 kPa. The compacted specimen of Kaolin soil exhibited a consistent collapse under all the studied inundation pressure. The collapse potential was observed to be increasing with an increase in the inundation pressure up to a maximum value of 13.85% under 800 kPa and then decreased to 11.7% under 1600 kPa. Microstructural analysis was carried out based on the fabric images and the pore size distributions (PSDs) obtained from FESEM analysis and mercury intrusion porosimetry (MIP), respectively. The PSDs and the soil fabric images of ‘as-compacted’ specimen and post-collapse specimen under 400 kPa were analyzed to understand the changes in the soil fabric and pores due to wetting. The pore size density curve for the post-collapse specimen was found to be on the finer side with respect to the ‘as-compacted’ specimen, indicating the reduction of the larger pores during the collapse. The inter-aggregate pores in the range of 0.1-0.5μm were identified as the major contributing pore size classes to the macroscopic volume change. Wetting under an inundation pressure results in the reduction of these pore sizes and lead to an increase in the finer pore sizes. The magnitude of inundation pressure influences the amount of reduction of these pores during the wetting process. The collapse potential was directly related to the degree of reduction in the pore volume contributed by these pore sizes.

Keywords: collapse behavior, inundation pressure, kaolin, microstructure

Procedia PDF Downloads 140

Authors: Humaira Athar, Brajeshwar Singh

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Generally, the brightness of the indoor environment of buildings is entirely maintained by the artificial lighting which has consumed a large amount of resources. It is reported that lighting consumes about 19% of the total generated electricity which accounts for about 30-40% of total energy consumption. One possible way is to reduce the lighting energy by exploiting sunlight either through the use of suitable devices or energy efficient materials like translucent concrete. Translucent concrete is one such architectural concrete which allows the passage of natural light as well as artificial light through it. Several attempts have been made on different aspects of translucent concrete such as light guiding materials (glass fibers, plastic fibers, cylinder etc.), concrete mix design and manufacturing methods for use as building elements. Concerns are, however, raised on various related issues such as poor compatibility between the optical fibers and cement paste, unaesthetic appearance due to disturbance occurred in the arrangement of fibers during vibration and high shrinkage in flowable concrete due to its high water/cement ratio. Need is felt to develop translucent concrete to meet the requirement of structural safety as OPC concrete with the maximized saving in energy towards the power of illumination and thermal load in buildings. Translucent concrete was produced using pre-treated plastic optical fibers (POF, 2mm dia.) and high slump white concrete. The concrete mix was proportioned in the ratio of 1:1.9:2.1 with a w/c ratio of 0.40. The POF was varied from 0.8-9 vol.%. The mechanical properties and light transmission of this concrete were determined. Thermal conductivity of samples was measured by a transient plate source technique. Daylight illumination was measured by a lux grid method as per BIS:SP-41. It was found that the compressive strength of translucent concrete increased with decreasing optical fiber content. An increase of ~28% in the compressive strength of concrete was noticed when fiber was pre-treated. FE-SEM images showed little-debonded zone between the fibers and cement paste which was well supported with pull-out bond strength test results (~187% improvement over untreated). The light transmission of concrete was in the range of 3-7% depending on fiber spacing (5-20 mm). The average daylight illuminance (~75 lux) was nearly equivalent to the criteria specified for illumination for circulation (80 lux). The thermal conductivity of translucent concrete was reduced by 28-40% with respect to plain concrete. The thermal load calculated by heat conduction equation was ~16% more than the plain concrete. Based on Design-Builder software, the total annual illumination energy load of a room using one side translucent concrete was 162.36 kW compared with the energy load of 249.75 kW for a room without concrete. The calculated energy saving on an account of the power of illumination was ~25%. A marginal improvement towards thermal comfort was also noticed. It is concluded that the translucent concrete has the advantages of the existing concrete (load bearing) with translucency and insulation characteristics. It saves a significant amount of energy by providing natural daylight instead of artificial power consumption of illumination.

Keywords: energy saving, light transmission, microstructure, plastic optical fibers, translucent concrete

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Authors: Olga Yu Kurapova, Alexander V. Shorokhov, Vladimir G. Konakov

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Nowadays, due to their exceptional anion conductivity at high temperatures cubic zirconia solid solutions, stabilized by rare-earth and alkaline-earth metal oxides, are widely used as a solid electrolyte (SE) materials in different electrochemical devices such as gas sensors, oxygen pumps, solid oxide fuel cells (SOFC), etc. Nowadays the intensive studies are carried out in a field of novel fully stabilized zirconia based SE development. The use of precursor powders for SE manufacturing allows predetermining the microstructure, electrical and sensor characteristics of zirconia based ceramics used as SE. Thus the goal of the present work was the investigation of the effect of precursor powder size on the electrical and sensor characteristics of fully stabilized zirconia-based solid electrolytes with compositions of 0,08Y2O3∙0,92ZrO2 (YSZ), 0,06Ce2O3∙ 0,06Y2O3∙0,88ZrO2 and 0,09Ce2O3∙0,06Y2O3-0,85ZrO2. The synthesis of precursors powders with different mean particle size was performed by sol-gel synthesis in the form of reversed co-precipitation from aqueous solutions. The cakes were washed until the neutral pH and pan-dried at 110 °С. Also, YSZ ceramics was obtained by conventional solid state synthesis including milling into a planetary mill. Then the powder was cold pressed into the pellets with a diameter of 7.2 and ~4 mm thickness at P ~16 kg/cm2 and then hydrostatically pressed. The pellets were annealed at 1600 °С for 2 hours. The phase composition of as-synthesized SE was investigated by X-Ray photoelectron spectroscopy ESCA (spectrometer ESCA-5400, PHI) X-ray diffraction analysis - XRD (Shimadzu XRD-6000). Following galvanic cell О2 (РО2(1)), Pt | SE | Pt, (РО2(2) = 0.21 atm) was used for SE sensor properties investigation. The value of РО2(1) was set by mixing of O2 and N2 in the defined proportions with the accuracy of  5%. The temperature was measured by Pt/Pt-10% Rh thermocouple, The cell electromotive force (EMF) measurement was carried out with ± 0.1 mV accuracy. During the operation at the constant temperature, reproducibility was better than 5 mV. Asymmetric potential measured for all SE appeared to be negligible. It was shown that the resistivity of YSZ ceramics decreases in about two times upon the mean agglomerates decrease from 200-250 to 40 nm. It is likely due to the both surface and bulk resistivity decrease in grains. So the overall decrease of grain size in ceramic SE results in the significant decrease of the total ceramics resistivity allowing sensor operation at lower temperatures. For the SE manufactured the estimation of oxygen ion transfer number tion was carried out in the range 600-800 °С. YSZ ceramics manufactured from powders with the mean particle size 40-140 nm, shows the highest values i.e. 0.97-0.98. SE manufactured from precursors with the mean particle size 40-140 nm shows higher sensor characteristic i.e. temperature and oxygen concentration EMF dependencies, EMF (ENernst - Ereal), tion, response time, then ceramics, manufactured by conventional solid state synthesis.

Keywords: oxygen sensors, precursor powders, sol-gel synthesis, stabilized zirconia ceramics

Procedia PDF Downloads 283

Authors: Alexia Wu, Joel Ribis, Jean-Christophe Brachet, Emmanuel Clouet, Benoit Arnal, Elodie Rouesne, Stéphane Urvoy, Justine Roubaud, Yves Serruys, Frederic Lepretre

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To enhance the safety of Light Water Reactor, accident tolerant fuel (ATF) claddings materials are under development. In the framework of CEA-AREVA-EDF collaborative program on ATF cladding materials, CEA has engaged specific studies on chromium coated zirconium alloys. Especially for Loss-of-Coolant-Accident situations, chromium coated claddings have shown some additional 'coping' time before achieving full embrittlement of the oxidized cladding, when compared to uncoated references – both tested in steam environment up to 1300°C. Nevertheless, the behavior of chromium coatings and the stability of the Zr-Cr interface under neutron irradiation remain unknown. Two main points are addressed: 1. Bulk Cr behavior under irradiation: Due to its BCC crystallographic structure, Cr is prone to Ductile-to-Brittle-Transition at quite high temperature. Irradiation could be responsible for a significant additional DBTT shift towards higher temperatures. 2. Zircaloy/Cr interface behavior under irradiation: Preliminary TEM examinations of un-irradiated samples revealed a singular Zircaloy-4/Cr interface with nanometric intermetallic phase layers. Such particular interfaces highlight questions of how they would behave under irradiation - intermetallic zirconium phases are known to be more or less stable under irradiations. Another concern is a potential enhancement of chromium diffusion into the zirconium-alpha based substrate. The purpose of this study is then to determine the behavior of such coatings after ion irradiations, as a surrogate to neutron irradiation. Ion irradiations were performed at the Jannus-Saclay facility (France). 20 MeV Kr8+ ions at 400°C with a flux of 2.8x1011 ions.cm-2.s-1 were used to irradiate chromium coatings of 1-2 µm thick on Zircaloy-4 sheets substrate. At the interface, the calculated damage is close to 10 dpa (SRIM, Quick Calculation Damage mode). Thin foil samples were prepared with FIB for both as-received and irradiated coated samples. Transmission Electron Microscopy (TEM) and in-situ tensile tests in a Scanning Electron Microscope are being used to characterize the un-irradiated and irradiated materials. High Resolution TEM highlights a great complexity of the interface before irradiation since it is formed of an alternation of intermetallic phases – C14 and C15. The interfaces formed by these intermetallic phases with chromium and zirconium show semi-coherency. Chemical analysis performed before irradiation shows some iron enrichment at the interface. The chromium coating bulk microstructures and properties are also studied before and after irradiation. On-going in-situ tensile tests focus on the capacity of chromium coatings to sustain some plastic deformation when tested up to 350°C. The stability of the Cr/Zr interface is shown after ion irradiation up to 10 dpa. This observation constitutes the first result after irradiation on these new coated claddings materials.

Keywords: accident tolerant fuel, HRTEM, interface, ion-irradiation

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Authors: Daniel Tscharnuter, Eliza Truszkiewicz, Gerald Pinter

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High-quality surfaces of plastic parts can be achieved in a very cost-effective manner using in-mold processes, where e.g. scratch resistant or high gloss polymer films are pre-formed and subsequently receive their support structure by injection molding. The pre-forming may be done by high-pressure forming. In this process, a polymer sheet is heated and subsequently formed into the mold by pressurized air. Due to the heat transfer to the cooled mold the polymer temperature drops below its glass transition temperature. This ensures that the deformed microstructure is retained after depressurizing, giving the sheet its final formed shape. The development of a forming process relies heavily on the experience of engineers and trial-and-error procedures. Repeated mold design and testing cycles are however both time- and cost-intensive. It is, therefore, desirable to study the process using reliable computer simulations. Through simulations, the construction of the mold and the effect of various process parameters, e.g. temperature levels, non-uniform heating or timing and magnitude of pressure, on the deformation of the polymer sheet can be analyzed. Detailed knowledge of the deformation is particularly important in the forming of polymer films with integrated electro-optical functions. Care must be taken in the placement of devices, sensors and electrical and optical paths, which are far more sensitive to deformation than the polymers. Reliable numerical prediction of the deformation of the polymer sheets requires sophisticated material models. Polymer films are often either transversely isotropic or orthotropic due to molecular orientations induced during manufacturing. The anisotropic behavior affects the resulting strain field in the deformed film. For example, parts of the same shape but different strain fields may be created by varying the orientation of the film with respect to the mold. The numerical simulation of the high-pressure forming of such films thus requires material models that can capture the nonlinear anisotropic mechanical behavior. There are numerous commercial polymer grades for the engineers to choose from when developing a new part. The effort required for comprehensive material characterization may be prohibitive, especially when several materials are candidates for a specific application. We, therefore, propose a class of models for compressible hyperelasticity, which may be determined from basic experimental data and which can capture key features of the mechanical response. Invariant-based hyperelastic models with a reduced number of invariants are formulated in a semi-numerical way, such that the models are determined from a single uniaxial tensile tests for isotropic materials, or two tensile tests in the principal directions for transversely isotropic or orthotropic materials. The simulation of the high pressure forming of an orthotropic polymer film is finally done using an orthotropic formulation of the hyperelastic model.

Keywords: hyperelastic, anisotropic, polymer film, thermoforming

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Authors: Ashok Kumar, Shiv Brat Singh, Kalyan Kumar Ray

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There is growing awareness to design steels against fatigue damage Ferrite martensite dual-phase steels are known to exhibit favourable mechanical properties like good strength, ductility, toughness, continuous yielding, and high work hardening rate. However, dual-phase steels containing bainite as second phase are potential alternatives for ferrite martensite steels for certain applications where good fatigue property is required. Fatigue properties of dual phase steels are popularly assessed by the nature of variation of crack growth rate (da/dN) with stress intensity factor range (∆K), and the magnitude of fatigue threshold (∆Kth) for long cracks. There exists an increased emphasis to understand not only the long crack fatigue behavior but also short crack growth behavior of ferrite bainite dual phase steels. The major objective of this report is to examine the influence of microstructures on the short and long crack growth behavior of a series of developed dual-phase steels with varying amounts of bainite and. Three low carbon steels containing Nb, Cr and Mo as microalloying elements steels were selected for making ferrite-bainite dual-phase microstructures by suitable heat treatments. The heat treatment consisted of austenitizing the steel at 1100°C for 20 min, cooling at different rates in air prior to soaking these in a salt bath at 500°C for one hour, and finally quenching in water. Tensile tests were carried out on 25 mm gauge length specimens with 5 mm diameter using nominal strain rate 0.6x10⁻³ s⁻¹ at room temperature. Fatigue crack growth studies were made on a recently developed specimen configuration using a rotating bending machine. The crack growth was monitored by interrupting the test and observing the specimens under an optical microscope connected to an Image analyzer. The estimated crack lengths (a) at varying number of cycles (N) in different fatigue experiments were analyzed to obtain log da/dN vs. log °∆K curves for determining ∆Kthsc. The microstructural features of these steels have been characterized and their influence on the near threshold crack growth has been examined. This investigation, in brief, involves (i) the estimation of ∆Kthsc and (ii) the examination of the influence of microstructure on short and long crack fatigue threshold. The maximum fatigue threshold values obtained from short crack growth experiments on various specimens of dual-phase steels containing different amounts of bainite are found to increase with increasing bainite content in all the investigated steels. The variations of fatigue behavior of the selected steel samples have been explained with the consideration of varying amounts of the constituent phases and their interactions with the generated microstructures during cyclic loading. Quantitative estimation of the different types of fatigue crack paths indicates that the propensity of a crack to pass through the interfaces depends on the relative amount of the microstructural constituents. The fatigue crack path is found to be predominantly intra-granular except for the ones containing > 70% bainite in which it is predominantly inter-granular.

Keywords: bainite, dual phase steel, fatigue crack growth rate, long crack fatigue threshold, short crack fatigue threshold

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Authors: Ali Ahmed Ali Al-Juboori, H. Zhu, D. Wexler, H. Li, C. Lu, J. McLeod, S. Pannila, J. Barnes

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A number of studies have focused on the formation mechanics of white etching layer and its origin in the railway operation. Until recently, the following hypotheses consider the precise mechanics of WELs formation: (i) WELs are the result of thermal process caused by wheel slip; (ii) WELs are mechanically induced by severe plastic deformation; (iii) WELs are caused by a combination of thermo-mechanical process. The mechanisms discussed above lead to occurrence of white etching layers on the area of wheel and rail contact. This is because the contact patch which is the active point of the wheel on the rail is exposed to highest shear stresses which result in localised severe plastic deformation; and highest rate of heat caused by wheel slipe during excessive traction or braking effort. However, if the WELs are not on the running band area, it would suggest that there is another cause of WELs formation. In railway system, particularly electrified railway, arcing phenomenon has been occurring more often and regularly on the rails. In electrified railway, the current is delivered to the train traction motor via contact wires and then returned to the station via the contact between the wheel and the rail. If the contact between the wheel and the rail is temporarily losing, due to dynamic vibration, entrapped dirt or water, lubricant effect or oxidation occurrences, high current can jump through the gap and results in arcing. The other resources of arcing also include the wheel passage the insulated joint and lightning on a train during bad weather. During the arcing, an extensive heat is generated and speared over a large area of top surface of rail. Thus, arcing is considered another heat source in the rail head (rather than wheel slipe) that results in microstructural changes and white etching layer formation. A head hardened (HH) rail steel, cut from a curved rail truck was used for the investigation. Samples were sectioned from a depth of 10 mm below the rail surface, where the material is considered to be still within the hardened layer but away from any microstructural changes on the top surface layer caused by train passage. These samples were subjected to electrical discharges by using Gas Tungsten Arc Welding (GTAW) machine. The arc current was controlled and moved along the samples surface in the direction of travel, as indicated by an arrow. Five different conditions were applied on the surface of the samples. Samples containing pre-existed WELs, taken from ex-service rail surface, were also considered in this study for comparison. Both simulated and ex-serviced WELs were characterised by advanced methods including SEM, TEM, TKD, EDS, XRD. Samples for TEM and TKFD were prepared by Focused Ion Beam (FIB) milling. The results showed that both simulated WELs by electrical arcing and ex-service WEL comprise similar microstructure. Brown etching layer was found with WELs and likely induced by a concurrent tempering process. This study provided a clear understanding of new formation mechanics of WELs which contributes to track maintenance procedure.

Keywords: white etching layer, arcing, brown etching layer, material characterisation

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Authors: O. Gsib, U. Peirera, C. Egles, S. A. Bencherif

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In skin regenerative medicine, one of the critical issues is to produce a three-dimensional scaffold with optimized porosity for dermal fibroblast infiltration and neovascularization, which exhibits high mechanical properties and displays sufficient wound healing characteristics. In this study, we report on the synthesis and characterization of macroporous sequential interpenetrating polymer networks (IPNs) combining skin wound healing properties of fibrin with the excellent physical properties of polyethylene glycol (PEG). Fibrin fibers serve as a provisional biologically active network to promote cell adhesion and proliferation while PEG provides the mechanical stability to maintain the entire 3D construct. After having modified both PEG and Serum Albumin (used for promoting enzymatic degradability) by adding methacrylate residues (PEGDM and SAM, respectively), Fibrin/PEGDM-SAM sequential IPNs were synthesized as follows: Macroporous sponges were first produced from PEGDM-SAM hydrogels by a freeze-drying technique and then rehydrated by adding the fibrin precursors. Environmental Scanning Electron Microscopy (ESEM) and Confocal Laser Scanning Microscopy (CLSM) were used to characterize their microstructure. Human dermal fibroblasts were cultivated during one week in the constructs and different cell culture parameters (viability, morphology, proliferation) were evaluated. Subcutaneous implantations of the scaffolds were conducted on five-week old male nude mice to investigate their biocompatibility in vivo. We successfully synthesized interconnected and macroporous Fibrin/PEGDM-SAM sequential IPNs. The viability of primary dermal fibroblasts was well maintained (above 90%) after 2 days of culture. Cells were able to adhere, spread and proliferate in the scaffolds suggesting the suitable porosity and intrinsic biologic properties of the constructs. The fibrin network adopted a spider web shape that covered partially the pores allowing easier cell infiltration into the macroporous structure. To further characterize the in vitro cell behavior, cell proliferation (EdU incorporation, MTS assay) is being studied. Preliminary histological analysis of animal studies indicated the persistence of hydrogels even after one-month post implantation and confirmed the absence of inflammation response, good biocompatibility and biointegration of our scaffolds within the surrounding tissues. These results suggest that our Fibrin/PEGDM-SAM IPNs could be considered as potential candidates for dermis regenerative medicine. Histological analysis will be completed to further assess scaffold remodeling including de novo extracellular matrix protein synthesis and early stage angiogenesis analysis. Compression measurements will be conducted to investigate the mechanical properties.

Keywords: fibrin, hydrogels for dermal reconstruction, polyethylene glycol, semi-interpenetrating polymer network

Procedia PDF Downloads 237

Authors: Jung-Il Suh, Hong-Gun Park, Jae-Eun Oh

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Recently, the use of long-span precast concrete (PC) construction has increased in modular construction such as storage buildings and parking facilities. When applying long span PC member, reducing weight of long span PC member should be conducted considering lifting capacity of crane and self-weight of PC member and use of structural lightweight concrete made by lightweight aggregate (LWA) can be considered. In the process of lightweight concrete production, segregation and bleeding could occur due to difference of specific gravity between cement (3.3) and lightweight aggregate (1.2~1.8) and reducing weight of binder is needed to prevent the segregation between binder and aggregate. Also, lightweight precast concrete made by cementitious materials such as fly ash and ground granulated blast furnace (GGBFS) which is lower than specific gravity of cement as a substitute for cement has been studied. When only using fly ash for cementless binder alkali-activation of fly ash is most important chemical process in which the original fly ash is dissolved by a strong alkaline medium in steam curing with high-temperature condition. Because curing condition is similar with environment of precast member production, additional process is not needed. Na-based chloride generally used as a strong alkali activator has a practical problem such as high pH toxicity and high manufacturing cost. Instead of Na-based alkali activator calcium hydroxide [Ca(OH)2] and sodium hydroxide [Na2CO3] might be used because it has a lower pH and less expensive than Na-based alkali activator. This study explored the influences on Ca(OH)2-Na2CO3-activated fly ash system in its microstructural aspects and strength and permeability using powder X-ray analysis (XRD), thermogravimetry (TGA), mercury intrusion porosimetry (MIP). On the basis of microstructural analysis, the conclusions are made as follows. Increase of Ca(OH)2/FA wt.% did not affect improvement of compressive strength. Also, Ca(OH)2/FA wt.% and Na2CO3/FA wt.% had little effect on specific gravity of saturated surface dry (SSD) and absolute dry (AD) condition to calculate water absorption. Especially, the binder is appropriate for structural lightweight concrete because specific gravity of the hardened paste has no difference with that of lightweight aggregate. The XRD and TGA/DTG results did not present considerable difference for the types and quantities of hydration products depending on w/b ratio, Ca(OH)2 wt.%, and Na2CO3 wt.%. In the case of higher molar quantity of Ca(OH)2 to Na2CO3, XRD peak indicated unreacted Ca(OH)2 while DTG peak was not presented because of small quantity. Thus, presence of unreacted Ca(OH)2 is too small quantity to effect on mechanical performance. As a result of MIP, the porosity volume related to capillary pore depends on the w/b ratio. In the same condition of w/b ratio, quantities of Ca(OH)2 and Na2CO3 have more influence on pore size distribution rather than total porosity. While average pore size decreased as Na2CO3/FA w.t% increased, the average pore size increased over 20 nm as Ca(OH)2/FA wt.% increased which has inverse proportional relationship between pore size and mechanical properties such as compressive strength and water permeability.

Keywords: Ca(OH)2, compressive strength, microstructure, fly ash, Na2CO3, water absorption

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Authors: Gianmarco Taveri, Ivo Dlouhy

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Geopolymers are well-suited materials to abate CO2 emission coming from the Portland cement production, and then replace them, in the near future, in building and other applications. The cost of production of geopolymers may be seen the only weakness, but the use of wastes as raw materials could provide a valid solution to this problem, as demonstrated by the successful incorporation of fly-ash, a by-product of thermal power plants, and waste glasses. Recycled glass in waste-derived geopolymers was lately employed as a further silica source. In this work we present, for the first time, the introduction of recycled borosilicate glass (BSG). BSG is actually a waste glass, since it derives from dismantled pharmaceutical vials and cannot be reused in the manufacturing of the original articles. Owing to the specific chemical composition (BSG is an ‘alumino-boro-silicate’), it was conceived to provide the key components of zeolitic networks, such as amorphous silica and alumina, as well as boria (B2O3), which may replace Al2O3 and contribute to the polycondensation process. The solid–state MAS NMR spectroscopy was used to assess the extent of boron oxide incorporation in the structure of geopolymers, and to define the degree of networking. FTIR spectroscopy was utilized to define the degree of polymerization and to detect boron bond vibration into the structure. Mechanical performance was tested by means of 3 point bending (flexural strength), chevron notch test (fracture toughness), compression test (compressive strength), micro-indentation test (Vicker’s hardness). Spectroscopy (SEM and Confocal spectroscopy) was performed on the specimens conducted to failure. FTIR showed a characteristic absorption band attributed to the stretching modes of tetrahedral boron ions, whose tetrahedral configuration is compatible to the reaction product of geopolymerization. 27Al NMR and 29Si NMR spectra were instrumental in understanding the extent of the reaction. 11B NMR spectroscopies evidenced a change of the trigonal boron (BO3) inside the BSG in favor of a quasi-total tetrahedral boron configuration (BO4). Thanks to these results, it was inferred that boron is part of the geopolymeric structure, replacing the Si in the network, similarly to the aluminum, and therefore improving the quality of the microstructure, in favor of a more cross-linked network. As expected, the material gained as much as 25% in compressive strength (45 MPa) compared to the literature, whereas no improvements were detected in flexural strength (~ 5 MPa) and superficial hardness (~ 78 HV). The material also exhibited a low fracture toughness (0.35 MPa*m1/2), with a tangible brittleness. SEM micrographies corroborated this behavior, showing a ragged surface, along with several cracks, due to the high presence of porosity and impurities, acting as preferential points for crack initiation. The 3D pattern of the surface fracture, following the confocal spectroscopy, evidenced an irregular crack propagation, whose proclivity was mainly, but not always, to follow the porosity. Hence, the crack initiation and propagation are largely unpredictable.

Keywords: borosilicate glass, characterization, fly-ash, geopolymerization

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Authors: Syfur Rahman, Mohammad J. Khattak

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Every year a huge quantity of recycling concrete aggregate (RCA) is generated in the United States of America. Utilization of RCA can solve the storage problem, prevent environmental pollution, and reduce the construction cost. However, due to the overall low strength and durability characteristics of RCA, its usages are limited to a certain area like a landfill, low strength base material, replacement of a few percentages of virgin aggregates in Portland cement concrete, etc. This study focuses on the improvement of the strength and durability characteristics of RCA by introducing the concept of roller-compacted geopolymer concrete. In this research, developed roller-compacted geopolymer concrete (RCGPC) and roller-compacted cement concrete (RCC) mixtures containing 100% recycled concrete aggregate were evaluated and compared. Several selected RCGPC mixtures were investigated to find out the effect of mixture variables, including sodium hydroxide (NaOH) molar concentration, sodium silicate (Na₂SiO₃), to sodium hydroxide (NaOH) ratio on the strength, stiffness and durability characteristics of the developed RCGPC. Sodium hydroxide (NaOH) and sodium silicate (Na₂SiO₃) were mixed in different ratios to synthesize the alkali activator. American Concrete Pavement Association (ACPA) recommended RCC gradation was used with a maximum nominal aggregate size of 19 mm with a 4% fine particle passing 0.075 mm sieve. The mixtures were made using NaOH molar concentration of 8M and 10M along with, Na₂SiO₃ to NaOH ratio of 0 and 1 by mass and 15% class F fly ash. Optimum alkali content and moisture content were determined for each RCGPC and RCC mixtures, respectively, using modified proctor test. Compressive strength, semi-circular bending beam strength, and dynamic modulus test were conducted to evaluate the mechanistic characteristics of both mixtures. To determine the optimum curing conditions for RCGPC, effects of different curing temperature and curing duration on compressive strength were also studied. Sulphate attack and freeze-thaw tests were also carried out to assess the durability properties of the developed mixtures. X-ray diffraction (XRD) was used for morphology and microstructure analysis. From the optimum moisture content results, it was found that RCGPC has high alkali content, which was mainly due to the high absorption capacity of RCA. It was found that the mixtures with Na₂SiO₃ to NaOH ratio of 1 yielded about 60% higher compressive strength than the ratio of 0. Further, the mixtures using 10M NaOH concentrations and alkali ratio of 1 produced about 28 MPa of compressive strength, which was around 33% higher than 8M NaOH mixtures. Similar results were obtained for elastic and dynamic modulus of the mixtures. On the other hand, the semi-circular bending beam strength remained the same for both 8 and 10 molar NaOH geopolymer mixtures. Formation of new geopolymeric compounds and chemical bonds in the newly formed novel RCGPC mixtures were also discovered using XRD analysis. The results of mechanical and durability testing further revealed that RCGPC performed similarly to that of RCC mixtures. Based on the results of mechanical and durability testing, the developed RCGPC mixtures using 100% recycled concrete could be used as a cost-effective solution for the construction of pavement structures.

Keywords: roller compacted concrete, geopolymer concrete, recycled concrete aggregate, concrete pavement, fly ash

Procedia PDF Downloads 138

Authors: R. P. Naik, A. K. Rakshit

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In recent years, with the rapid development in science and technology, people have increasing requirements on uses of clothing for new functions, which contributes to opportunities for further development and incorporation of new technologies along with novel materials. In this context, textiles are of fast decalescence or fast heat radiation media as per as comfort accountability of textile articles are concern. The microstructure and texture of textiles play a vital role in determining the heat-moisture comfort level of the human body because clothing serves as a barrier to the outside environment and a transporter of heat and moisture from the body to the surrounding environment to keep thermal balance between body heat produced and body heat loss. The main bottleneck which is associated with textile materials to be successful as thermal insulation materials can be enumerated as; firstly, high loft or bulkiness of material so as to provide predetermined amount of insulation by ensuring sufficient trapping of air. Secondly, the insulation depends on forced convection; such convective heat loss cannot be prevented by textile material. Third is that the textile alone cannot reach the level of thermal conductivity lower than 0.025 W/ m.k of air. Perhaps, nano-fibers can do so, but still, mass production and cost-effectiveness is a problem. Finally, such high loft materials for thermal insulation becomes heavier and uneasy to manage especially when required to carry over a body. The proposed works aim at developing lightweight effective thermal insulation textiles in combination with nanoporous silica-gel which provides the fundamental basis for the optimization of material properties to achieve good performance of the clothing system. This flexible nonwoven silica-gel composites fabric in intact monolith was successfully developed by reinforcing SiO2-gel in thermal bonded nonwoven fabric via sol-gel processing. Ambient Pressure Drying method is opted for silica gel preparation for cost-effective manufacturing. The formed structure of the nonwoven / SiO₂ -gel composites were analyzed, and the transfer properties were measured. The effects of structure and fibre on the thermal properties of the SiO₂-gel composites were evaluated. Samples are then tested against untreated samples of same GSM in order to study the effect of SiO₂-gel application on various properties of nonwoven fabric. The nonwoven fabric composites reinforced with aerogel showed intact monolith structure were also analyzed for their surface structure, functional group present, microscopic images. Developed product reveals a significant reduction in pores' size and air permeability than the conventional nonwoven fabric. Composite made from polyester fibre with lower GSM shows lowest thermal conductivity. Results obtained were statistically analyzed by using STATISTICA-6 software for their level of significance. Univariate tests of significance for various parameters are practiced which gives the P value for analyzing significance level along with that regression summary for dependent variable are also studied to obtain correlation coefficient.

Keywords: silica-gel, heat insulation, nonwoven fabric, thermal barrier clothing

Procedia PDF Downloads 112

Authors: Linmin Zhang

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Entrained-flow gasification technology is considered the most promising gasification technology because of its clean and efficient utilization characteristics. The stable fluidity of slag at high temperatures is the key to affecting the long-period operation of the gasifier. The diversity and differences of coal ash-slag systems make it difficult to meet the requirements for stable slagging in entrained-flow gasifiers. Therefore, coal blending or adding fluxes has been used in industry for a long time to improve the flow behavior of coal ash. As a by-product of the indirect coal liquefaction process, indirect coal liquefaction residue (ICLR) is a kind of industrial solid waste that is usually disposed of by stacking or landfilling. However, this disposal method will not only occupy land resources but also cause serious pollution to soil and water bodies by leachate containing toxic and harmful metals. As a carbon-containing matrix, ICLR is not only a kind of waste but also a kind of energy substance. Utilizing existing industrial gasifiers to blend combustion ICLR can not only transform industrial solid waste into fuel but also save coal resources. Moreover, the ICLR usually contains a unique ash chemical composition different from coal, which will affect the slagging performance of the gasifier. Therefore, exploring the effect of the ash addition in ICLR on the coal ash flow behavior can not only improve the slagging performance and gasification efficiency of entrained-flow gasifier by using the unique ash chemical composition of ICLR but also provide some theoretical support for the large-scale consumption of industrial solid waste. Combining molecular dynamics simulation with Raman spectroscopy experiment, the effect of ICLR addition on slag structure and fluidity was explained, and the relationship between the evolution law of slag short/medium range microstructure and macroscopic flow behavior was discussed. The research found that the high silicon and aluminum content in coal ash led to the formation of complex [SiO₄]⁴- tetrahedron and [AlO₄]⁵- tetrahedron structures at high temperature, and the [SiO₄]⁴- tetrahedron and [AlO₄]⁵- tetrahedron were connected by oxygen atoms to form a multi-membered ring structure with high polymerization degree. Due to the action of the multi-membered ring structure, the internal friction in the slag increased, and the viscosity value was higher on the macro-level. As a network-modified ion, Fe2+ could replace Si4+ and Al3+ in the multi-membered ring structure and combine with O2-, which will destroy the bridge oxygen (BO) structure and transform more complex tri cluster oxygen (TO) and bridge oxygen (BO) into simple non-bridge oxygen (NBO) structure. As a result, a large number of multi-membered rings with high polymerization degrees were depolymerized into low-membered rings with low polymerization degrees. The evolution of oxygen types and ring structures in slag reduced the structure complexity and polymerization degree of coal ash slag, resulting in a decrease in the viscosity of coal ash slag.

Keywords: ash slag, coal gasification, fluidity, industrial solid waste, slag structure

Procedia PDF Downloads 31

Authors: Marta Malo, Carlota Soto, Carmen García-Rosales, Teresa Hernández

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SiC based composites are candidates for possible use as structural and functional materials in the future fusion reactors, the main role is intended for the blanket modules. In the blanket, the neutrons produced in the fusion reaction slow down and their energy is transformed into heat in order to finally generate electrical power. In the blanket design named Dual Coolant Lead Lithium (DCLL), a PbLi alloy for power conversion and tritium breeding circulates inside hollow channels called Flow Channel Inserts (FCIs). These FCI must protect the steel structures against the highly corrosive PbLi liquid and the high temperatures, but also provide electrical insulation in order to minimize magnetohydrodynamic interactions of the flowing liquid metal with the high magnetic field present in a magnetically confined fusion environment. Due to their nominally high temperature and radiation stability as well as corrosion resistance, SiC is the main choice for the flow channel inserts. The significantly lower manufacturing cost presents porous SiC (dense coating is required in order to assure protection against corrosion and as a tritium barrier) as a firm alternative to SiC/SiC composites for this purpose. This application requires the materials to be exposed to high radiation levels and extreme temperatures, conditions for which previous studies have shown noticeable changes in both the microstructure and the electrical properties of different types of silicon carbide. Both initial properties and radiation/temperature induced damage strongly depend on the crystal structure, polytype, impurities/additives that are determined by the fabrication process, so the development of a suitable material requires full control of these variables. For this work, several SiC samples with different percentage of porosity and sintering additives have been manufactured by the so-called sacrificial template method at the Ceit-IK4 Technology Center (San Sebastián, Spain), and characterized at Ciemat (Madrid, Spain). Electrical conductivity was measured as a function of temperature before and after irradiation with 1.8 MeV electrons in the Ciemat HVEC Van de Graaff accelerator up to 140 MGy (~ 2·10 -5 dpa). Radiation-induced conductivity (RIC) was also examined during irradiation at 550 ºC for different dose rates (from 0.5 to 5 kGy/s). Although no significant RIC was found in general for any of the samples, electrical conductivity increase with irradiation dose was observed to occur for some compositions with a linear tendency. However, first results indicate enhanced radiation resistance for coated samples. Preliminary thermogravimetric tests of selected samples, together with posterior XRD analysis allowed interpret radiation-induced modification of the electrical conductivity in terms of changes in the SiC crystalline structure. Further analysis is needed in order to confirm this.

Keywords: DCLL blanket, electrical conductivity, flow channel insert, porous SiC, radiation damage, thermal stability

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Authors: Mohammad M. Khan, Pankaj Agarwal

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The present investigation deals with the microstructures, mechanical and detailed wear characteristics of in situ TiC particles reinforced zinc aluminum-based metal matrix composites. The composites have been synthesized by liquid metallurgy route using vortex technique. The composite was found to be harder than the matrix alloy due to high hardness of the dispersoid particles therein. The former was also lower in ultimate tensile strength and ductility as compared to the matrix alloy. This could be explained to be due to the use of coarser size dispersoid and larger interparticle spacing. Reasonably uniform distribution of the dispersoid phase in the alloy matrix and good interfacial bonding between the dispersoid and matrix was observed. The composite exhibited predominantly brittle mode of fracture with microcracking in the dispersoid phase indicating effective easy transfer of load from matrix to the dispersoid particles. To study the wear behavior of the samples three different types of tests were performed namely: (i) sliding wear tests using a pin on disc machine under dry condition, (ii) high stress (two-body) abrasive wear tests using different combinations of abrasive media and specimen surfaces under the conditions of varying abrasive size, traversal distance and load, and (iii) low-stress (three-body) abrasion tests using a rubber wheel abrasion tester at various loads and traversal distances using different abrasive media. In sliding wear test, significantly lower wear rates were observed in the case of base alloy over that of the composites. This has been attributed to the poor room temperature strength as a result of increased microcracking tendency of the composite over the matrix alloy. Wear surfaces of the composite revealed the presence of fragmented dispersoid particles and microcracking whereas the wear surface of matrix alloy was observed to be smooth with shallow grooves. During high-stress abrasion, the presence of the reinforcement offered increased resistance to the destructive action of the abrasive particles. Microcracking tendency was also enhanced because of the reinforcement in the matrix. The negative effect of the microcracking tendency was predominant by the abrasion resistance of the dispersoid. As a result, the composite attained improved wear resistance than the matrix alloy. The wear rate increased with load and abrasive size due to a larger depth of cut made by the abrasive medium. The wear surfaces revealed fine grooves, and damaged reinforcement particles while subsurface regions revealed limited plastic deformation and microcracking and fracturing of the dispersoid phase. During low-stress abrasion, the composite experienced significantly less wear rate than the matrix alloy irrespective of the test conditions. This could be explained to be due to wear resistance offered by the hard dispersoid phase thereby protecting the softer matrix against the destructive action of the abrasive medium. Abraded surfaces of the composite showed protrusion of dispersoid phase. The subsurface regions of the composites exhibited decohesion of the dispersoid phase along with its microcracking and limited plastic deformation in the vicinity of the abraded surfaces.

Keywords: abrasive wear, liquid metallurgy, metal martix composite, SEM

Procedia PDF Downloads 152

Authors: Marta Paszkiewicz, Justyna Łuczak, Martyna Marchelek, Adriana Zaleska-Medynska

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In recent years, photocatalytical processes have been intensively investigated for destruction of pollutants, hydrogen evolution, disinfection of water, air and surfaces, for the construction of self-cleaning materials (tiles, glass, fibres, etc.). Titanium dioxide (TiO2) is the most popular material used in heterogeneous photocatalysis due to its excellent properties, such as high stability, chemical inertness, non-toxicity and low cost. It is well known that morphology and microstructure of TiO2 significantly influence the photocatalytic activity. This characteristics as well as other physical and structural properties of photocatalysts, i.e., specific surface area or density of crystalline defects, could be controlled by preparation route. In this regard, TiO2 particles can be obtained by sol-gel, hydrothermal, sonochemical methods, chemical vapour deposition and alternatively, by ionothermal synthesis using ionic liquids (ILs). In the TiO2 particles synthesis ILs may play a role of a solvent, soft template, reagent, agent promoting reduction of the precursor or particles stabilizer during synthesis of inorganic materials. In this work, the effect of the ILs anion type on morphology and photoactivity of TiO2 is presented. The preparation of TiO2 microparticles with spherical structure was successfully achieved by solvothermal method, using tetra-tert-butyl orthotitatane (TBOT) as the precursor. The reaction process was assisted by an ionic liquids 1-butyl-3-methylimidazolium bromide [BMIM][Br], 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF4] and 1-butyl-3-methylimidazolium haxafluorophosphate [BMIM][PF6]. Various molar ratios of all ILs to TBOT (IL:TBOT) were chosen. For comparison, reference TiO2 was prepared using the same method without IL addition. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Brenauer-Emmett-Teller surface area (BET), NCHS analysis, and FTIR spectroscopy were used to characterize the surface properties of the samples. The photocatalytic activity was investigated by means of phenol photodegradation in the aqueous phase as a model pollutant, as well as formation of hydroxyl radicals based on detection of fluorescent product of coumarine hydroxylation. The analysis results showed that the TiO2 microspheres had spherical structure with the diameters ranging from 1 to 6 µm. The TEM micrographs gave a bright observation of the samples in which the particles were comprised of inter-aggregated crystals. It could be also observed that the IL-assisted TiO2 microspheres are not hollow, which provides additional information about possible formation mechanism. Application of the ILs results in rise of the photocatalytic activity as well as BET surface area of TiO2 as compared to pure TiO2. The results of the formation of 7-hydroxycoumarin indicated that the increased amount of ·OH produced at the surface of excited TiO2 for samples TiO2_ILs well correlated with more efficient degradation of phenol. NCHS analysis showed that ionic liquids remained on the TiO2 surface confirming structure directing role of that compounds.

Keywords: heterogeneous photocatalysis, IL-assisted synthesis, ionic liquids, TiO2

Procedia PDF Downloads 268

Authors: D. Ficai, A. Ficai, D. Gudovan, I. A. Gudovan, I. Ardelean, R. Trusca, E. Andronescu, V. Mitran, A. Cimpean

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In the last years, scientists struggled hardly to mimic bone structures to develop implants and biostructures which present higher biocompatibility and reduced rejection rate. One way to obtain this goal is to use similar materials as that of bone, namely collagen/hydroxyapatite composite materials. However, it is very important to tailor both compositions but also the microstructure of the bone that would ensure both the optimal osteointegartion and the mechanical properties required by the application. In this study, new collagen/hydroxyapatites composite materials doped with Cu, Li, Mn, Zn were successfully prepared. The synthesis method is described below: weight the Ca(OH)₂ mass, i.e., 7,3067g, and ZnCl₂ (0.134g), CuSO₄ (0.159g), LiCO₃ (0.133g), MnCl₂.4H₂O (0.1971g), and suspend in 100ml distilled water under magnetic stirring. The solution thus obtained is added a solution of NaH₂PO₄*H2O (8.247g dissolved in 50ml distilled water) under slow dropping of 1 ml/min followed by adjusting the pH to 9.5 with HCl and finally filter and wash until neutral pH. The as-obtained slurry was dried in the oven at 80°C and then calcined at 600°C in order to ensure a proper purification of the final product of organic phases, also inducing a proper sterilization of the mixture before insertion into the collagen matrix. The collagen/hydroxyapatite composite materials are tailored from morphological point of view to optimize their biocompatibility and bio-integration against mechanical properties whereas the addition of the dopants is aimed to improve the biological activity of the samples. The addition of transitional metals can improve the biocompatibility and especially the osteoblasts adhesion (Mn²⁺) or to induce slightly better osteoblast differentiation of the osteoblast, Zn²⁺ being a cofactor for many enzymes including those responsible for cell differentiation. If the amount is too high, the final material can become toxic and lose all of its biocompatibility. In order to achieve a good biocompatibility and not reach the cytotoxic effect, the amount of transitional metals added has to be maintained at low levels (0.5% molar). The amount of transitional metals entering into the elemental cell of HA will be verified using inductively-coupled plasma mass spectrometric system. This highly sensitive technique is necessary, because, at such low levels of transitional metals, the difference between biocompatible and cytotoxic is a very thin line, thus requiring proper and thorough investigation using a precise technique. In order to determine the structure and morphology of the obtained composite materials, IR spectroscopy, X-Ray diffraction (XRD), scanning electron microscopy (SEM), and Energy Dispersive X-Ray Spectrometry (EDS) were used. Acknowledgment: The present work was possible due to the EU-funding grant POSCCE-A2O2.2.1-2013-1, Project No. 638/12.03.2014, code SMIS-CSNR 48652. The financial contribution received from the national project “Biomimetic porous structures obtained by 3D printing developed for bone tissue engineering (BIOGRAFTPRINT), No. 127PED/2017 is also highly acknowledged.

Keywords: collagen, composite materials, hydroxyapatite, bone tissue engineering

Procedia PDF Downloads 207

Authors: O. Squillace, R. L. Thompson

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Migration of small molecules to, and across the surface of polymer matrices is a little-studied problem with important industrial applications. Tackifiers in adhesives, flavors in foods and binding agents in paints all present situations where the function of a product depends on the ability of small molecules to migrate through a polymer matrix to achieve the desired properties such as softness, dispersion of fillers, and to deliver an effect that is felt (or tasted) on a surface. It’s been shown that the chemical and molecular structure, surface free energies, phase behavior, close environment and compatibility of the system, influence the migrants’ motion. When differences in behavior, such as occurrence of segregation to the surface or not, are observed it is then of crucial importance to identify and get a better understanding of the driving forces involved in the process of molecular migration. In this aim, experience is meant to be allied with theory in order to deliver a validated theoretical and computational toolkit to describe and predict these phenomena. The systems that have been chosen for this study aim to address the effect of polarity mismatch between the migrants and the polymer matrix and that of a second migrant over the first one. As a non-polar resin polymer, polyvinyl acetate is used as the material to which more or less polar migrants (sorbitol, carvone, octanoic acid (OA), triacetin) are to be added. Through contact angle measurement a surface excess is seen for sorbitol (polar) mixed with PVAc as the surface energy is lowered compare to the one of pure PVAc. This effect is increased upon the addition of carvon or triacetin (non-polars). Surface micro-structures are also evidenced by atomic force microscopy (AFM). Ion beam analysis (Nuclear Reaction Analysis), supplemented by neutron reflectometry can accurately characterize the self-organization of surfactants, oligomers, aromatic molecules in polymer films in order to relate the macroscopic behavior to the length scales that are amenable to simulation. The nuclear reaction analysis (NRA) data for deuterated OA 20% shows the evidence of a surface excess which is enhanced after annealing. The addition of 10% triacetin, as a second migrant, results in the formation of an underlying layer enriched in triacetin below the surface excess of OA. The results show that molecules in polarity mismatch with the matrix tend to segregate to the surface, and this is favored by the addition of a second migrant of the same polarity than the matrix. As studies have been restricted to materials that are model supported films under static conditions in a first step, it is also wished to address the more challenging conditions of materials under controlled stress or strain. To achieve this, a simple rig and PDMS cell have been designed to stretch the material to a defined strain and to probe these mechanical effects by ion beam analysis and atomic force microscopy. This will make a significant step towards exploring the influence of extensional strain on surface segregation, flavor release in cross-linked rubbers.

Keywords: polymers, surface segregation, thin films, molecular migration

Procedia PDF Downloads 134

Authors: Kamolvara Sirisuksakulchai, Soamwadee Chaianansutcharit, Kazunori Sato

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Solid Oxide Fuel Cells (SOFCs) have been considered as one of the most efficient large unit power generators for household and industrial applications. The efficiency of an electronic cell depends mainly on the electrochemical reactions in the anode. The development of anode materials has been intensely studied to achieve higher kinetic rates of redox reactions and lower internal resistance. Recent studies have introduced an efficient cermet (ceramic-metallic) material for its ability in fuel oxidation and oxide conduction. This could expand the reactive site, also known as the triple-phase boundary (TPB), thus increasing the overall performance. In this study, a bimetallic catalyst Ni₀.₇₅Co₀.₂₅Oₓ was combined with Gd₀.₁Ce₀.₉O₁.₉₅ (GDC) to be used as a cermet anode (NiCo-GDC) for an anode-supported type SOFC. The synthesis of Ni₀.₇₅Co₀.₂₅Oₓ was carried out by ball milling NiO and Co3O4 powders in ethanol and calcined at 1000 °C. The Gd₀.₁Ce₀.₉O₁.₉₅ was prepared by a urea co-precipitation method. Precursors of Gd(NO₃)₃·6H₂O and Ce(NO₃)₃·6H₂O were dissolved in distilled water with the addition of urea and were heated subsequently. The heated mixture product was filtered and rinsed thoroughly, then dried and calcined at 800 °C and 1500 °C, respectively. The two powders were combined followed by pelletization and sintering at 1100 °C to form an anode support layer. The fabrications of an electrolyte layer and cathode layer were conducted. The electrochemical performance in H₂ was measured from 800 °C to 600 °C while for CH₄ was from 750 °C to 600 °C. The maximum power density at 750 °C in H₂ was 13% higher than in CH₄. The difference in performance was due to higher polarization resistances confirmed by the impedance spectra. According to the standard enthalpy, the dissociation energy of C-H bonds in CH₄ is slightly higher than the H-H bond H₂. The dissociation of CH₄ could be the cause of resistance within the anode material. The results from lower temperatures showed a descending trend of power density in relevance to the increased polarization resistance. This was due to lowering conductivity when the temperature decreases. The long-term stability was measured at 750 °C in CH₄ monitoring at 12-hour intervals. The maximum power density tends to increase gradually with time while the resistances were maintained. This suggests the enhanced stability from charge transfer activities in doped ceria due to the transition of Ce⁴⁺ ↔ Ce³⁺ at low oxygen partial pressure and high-temperature atmosphere. However, the power density started to drop after 60 h, and the cell potential also dropped from 0.3249 V to 0.2850 V. These phenomena was confirmed by a shifted impedance spectra indicating a higher ohmic resistance. The observation by FESEM and EDX-mapping suggests the degradation due to mass transport of ions in the electrolyte while the anode microstructure was still maintained. In summary, the electrochemical test and stability test for 60 h was achieved by NiCo-GDC cermet anode. Coke deposition was not detected after operation in CH₄, hence this confirms the superior properties of the bimetallic cermet anode over typical Ni-GDC.

Keywords: bimetallic catalyst, ceria-based SOFCs, methane oxidation, solid oxide fuel cell

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Authors: Ece A. Irmak, Amdulla O. Mekhrabov, M. Vedat Akdeniz

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There is a growing interest on the synthesis and characterization of nanoalloys since the unique chemical, and physical properties of nanoalloys can be tuned and, consequently, new structural motifs can be created by varying the type of constituent elements, atomic and magnetic ordering, as well as size and shape of the nanoparticles. Due to the fine size effects, magnetic nanoalloys have considerable attention with their enhanced mechanical, electrical, optical and magnetic behavior. As an important magnetic nanoalloy, the novel application area of Fe-Ni based nanoalloys is expected to be widened in the chemical, aerospace industry and magnetic biomedical applications. Noble metals have been using in biomedical applications for several years because of their surface plasmon properties. In this respect, iron-nickel nanoalloys are promising materials for magnetic biomedical applications because they show novel properties such as superparamagnetism and surface plasmon resonance property. Also, there is great attention for the usage Fe-Ni based nanoalloys as radar absorbing materials in aerospace and stealth industry due to having high Curie temperature, high permeability and high saturation magnetization with good thermal stability. In this study, FeNi₃ bimetallic nanoalloys were synthesized by mechanical alloying in a planetary high energy ball mill. In mechanical alloying, micron size powders are placed into the mill with milling media. The powders are repeatedly deformed, fractured and alloyed by high energy collision under the impact of balls until the desired composition and particle size is achieved. The experimental studies were carried out in two parts. Firstly, dry mechanical alloying with high energy dry planetary ball milling was applied to obtain FeNi₃ nanoparticles. Secondly, dry milling was followed by surfactant-assisted ball milling to observe the surfactant and solvent effect on the structure, size, and properties of the FeNi₃ nanoalloys. In the first part, the powder sample of iron-nickel was prepared according to the 1:3 iron to nickel ratio to produce FeNi₃ nanoparticles and the 1:10 powder to ball weight ratio. To avoid oxidation during milling, the vials had been filled with Ar inert gas before milling started. The powders were milled for 80 hours in total and the synthesis of the FeNi₃ intermetallic nanoparticles was succeeded by mechanical alloying in 40 hours. Also, regarding the particle size, it was found that the amount of nano-sized particles raised with increasing milling time. In the second part of the study, dry milling of the Fe and Ni powders with the same stoichiometric ratio was repeated. Then, to prevent agglomeration and to obtain smaller sized nanoparticles with superparamagnetic behavior, surfactants and solvent are added to the system, after 40-hour milling time, with the completion of the mechanical alloying. During surfactant-assisted ball milling, heptane was used as milling medium, and as surfactants, oleic acid and oleylamine were used in the high energy ball milling processes. The characterization of the alloyed particles in terms of microstructure, morphology, particle size, thermal and magnetic properties with respect to milling time was done by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, vibrating-sample magnetometer, and differential scanning calorimetry.

Keywords: iron-nickel systems, magnetic nanoalloys, mechanical alloying, nanoalloy characterization, surfactant-assisted ball milling

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Authors: Łukasz Mazur, Kamil Domaradzki, Maciej Bik, Tomasz Brylewski, Aleksander Gil

Abstract:

Interconnects used in solid oxide fuel and electrolyzer cells (SOFCₛ/SOECs) serve several important functions, and therefore interconnect materials must exhibit certain properties. Their thermal expansion coefficient needs to match that of the ceramic components of these devices – the electrolyte, anode and cathode. Interconnects also provide structural rigidity to the entire device, which is why interconnect materials must exhibit sufficient mechanical strength at high temperatures. Gas-tightness is also a prerequisite since they separate gas reagents, and they also must provide very good electrical contact between neighboring cells over the entire operating time. High-chromium ferritic steels meets these requirements to a high degree but are affected by the formation of a Cr₂O₃ scale, which leads to increased electrical resistance. The final criterion for interconnect materials is chemical inertness in relation to the remaining cell components. In the case of ferritic steels, this has proved difficult due to the formation of volatile and reactive oxyhydroxides observed when Cr₂O3 is exposed to oxygen and water vapor. This process is particularly harmful on the cathode side in SOFCs and the anode side in SOECs. To mitigate this, protective-conducting ceramic coatings can be deposited on an interconnect's surface. The area-specific resistance (ASR) of a single interconnect cannot exceed 0.1 m-2 at any point of the device's operation. The rate at which the CrO₃ scale grows on ferritic steels can be reduced significantly via the so-called reactive element effect (REE). Research has shown that the deposition of Gd₂O₃ nanoparticles on the surface of the Crofer 22 APU, already modified using a protective-conducting spinel layer, further improves the oxidation resistance of this steel. However, the deposition of the manganese-cobalt spinel layer is a rather complex process and is performed at high temperatures in reducing and oxidizing atmospheres. There was thus reason to believe that this process may reduce the effectiveness of Gd₂O₃ nanoparticles added as an active element source. The objective of the present study was, therefore, to determine any potential impact by introducing a preoxidation stage after the nanoparticle deposition and before the steel is coated with the spinel. This should have allowed the nanoparticles to incorporate into the interior of the scale formed on the steel. Different samples were oxidized for 7000 h in air at 1073 K under quasi-isothermal conditions. The phase composition, chemical composition, and microstructure of the oxidation products formed on the samples were determined using X-ray diffraction, Raman spectroscopy, and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy. A four-point, two-probe DC method was applied to measure ASR. It was found that coating deposition does indeed reduce the beneficial effect of Gd₂O₃ addition, since the smallest mass gain and the lowest ASR value were determined for the sample for which the additional preoxidation stage had been performed. It can be assumed that during this stage, gadolinium incorporates into and segregates at grain boundaries in the thin Cr₂O₃ that is forming. This allows the Gd₂O₃ nanoparticles to be a more effective source of the active element.

Keywords: interconnects, oxide nanoparticles, reactive element effect, SOEC, SOFC

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Authors: Ivan Maguire, Alan Barrett, Alex Forte, Sandra Kwiatkowska, Rohit Mishra, Jens Ducrèe, Fiona Regan

Abstract:

Biofouling is defined as the gradual accumulation of Biomimetics refers to the use and imitation of principles copied from nature. Biomimetics has found interest across many commercial disciplines. Among many biological objects and their functions, aquatic animals deserve a special attention due to their antimicrobial capabilities resulting from chemical composition, surface topography or other behavioural defences, which can be used as an inspiration for antifouling technology. Marine biofouling has detrimental effects on seagoing vessels, both commercial and leisure, as well as on oceanographic sensors, offshore drilling rigs, and aquaculture installations. Sensor optics, membranes, housings and platforms can become fouled leading to problems with sensor performance and data integrity. While many anti-fouling solutions are currently being investigated as a cost-cutting measure, biofouling settlement may also be prevented by creating a surface that does not satisfy the settlement conditions. Brill (Scophthalmus rhombus) is a small flatfish occurring in marine waters of Mediterranean as well as Norway and Iceland. It inhabits sandy and muddy coastal waters from 5 to 80 meters. Its skin colour changes depending on environment, but generally is brownish with light and dark freckles, with creamy underside. Brill is oval in shape and its flesh is white. The aim of this study is to translate the unique micro-topography of the brill scale, to design marine inspired biomimetic surface coating and test it against a typical fouling organism. Following extensive study of scale topography of the brill fish (Scophthalmus rhombus) and the settlement behaviour of the diatom species Psammodictyon sp. via SEM, two state-of-the-art antifouling surface solutions were designed and investigated; A brill fish scale bioinspired surface pattern platform (BFD), and generic and uniformly-arrayed, circular micropillar platform (MPD), with offsets based on diatom species settlement behaviour. The BFD approach consists of different ~5 μm by ~90 μm Brill-replica patterns, grown to a 5 μm height, in a linear array pattern. The MPD approach utilises hexagonal-packed cylindrical pillars 10.6 μm in diameter, grown to a height of 5 μm, with vertical offset of 15 μm and horizontal offset of 26.6 μm. Photolithography was employed for microstructure growth, with a polydimethylsiloxane (PDMS) chip-based used as a testbed for diatom adhesion on both platforms. Settlement and adhesion tests were performed using this PDMS microfluidic chip through subjugation to centrifugal force via an in-house developed ‘spin-stand’ which features a motor, in combination with a high-resolution camera, for real-time observing diatom release from PDMS material. Diatom adhesion strength can therefore be determined based on the centrifugal force generated at varying rotational speeds. It is hoped that both the replica and bio-inspired solutions will give comparable anti-fouling results to these synthetic surfaces, whilst also assisting in determining whether anti-fouling solutions should predominantly be investigating either fully bioreplica-based, or a bioinspired, synthetically-based design.

Keywords: anti-fouling applications, bio-inspired microstructures, centrifugal microfluidics, surface modification

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Authors: Łukasz Mazur, Kamil Domaradzki, Bartosz Kamecki, Justyna Ignaczak, Sebastian Molin, Aleksander Gil, Tomasz Brylewski

Abstract:

The rising global power consumption necessitates the development of new energy storage solutions. Prospective technologies include solid oxide electrolyzer cells (SOECs), which convert surplus electrical energy into hydrogen. An electrolyzer cell consists of a porous anode, and cathode, and a dense electrolyte. Power output is increased by connecting cells into stacks using interconnects. Interconnects are currently made from high-chromium ferritic steels – for example, Crofer 22 APU – which exhibit high oxidation resistance and a thermal expansion coefficient that is similar to that of electrode materials. These materials have one disadvantage – their area-specific resistance (ASR) gradually increases due to the formation of a Cr₂O₃ scale on their surface as a result of oxidation. The chromia in the scale also reacts with the water vapor present in the reaction media, forming volatile chromium oxyhydroxides, which in turn react with electrode materials and cause their deterioration. The electrochemical efficiency of SOECs thus decreases. To mitigate this, the interconnect surface can be modified with protective-conducting coatings of spinel or other materials. The high prices of SOEC components -especially the Crofer 22 APU- have prevented their widespread adoption. More inexpensive counterparts, therefore, need to be found, and their properties need to be enhanced to make them viable. Candidates include the Nirosta 4016/1,4016 low-chromium ferritic steel with a chromium content of just 16.3 wt%. This steel's resistance to high-temperature oxidation was improved by depositing Gd₂O₃ nanoparticles on its surface via either dip coating or electrolysis. Modification with CeO₂ or Ce₀.₉Y₀.₁O₂ nanoparticles deposited by means of spray pyrolysis was also tested. These methods were selected because of their low cost and simplicity of application. The aim of this study was to investigate the oxidation kinetics of Nirosta 4016/1,4016 modified using the afore-mentioned methods and to subsequently measure the obtained samples' ASR. The samples were oxidized for 100 h in the air as well as air/H₂O and Ar/H₂/H₂O mixtures at 1073 K. Such conditions reflect those found in the anode and cathode operating space during real-life use of SOECs. Phase and chemical composition and the microstructure of oxidation products were determined using XRD and SEM-EDS. ASR was measured over the range of 623-1073 K using a four-point, two-probe DC technique. The results indicate that the applied nanoparticles improve the oxidation resistance and electrical properties of the studied layered systems. The properties of individual systems varied significantly depending on the applied reaction medium. Gd₂O₃ nanoparticles improved oxidation resistance to a greater degree than either CeO₂ or Ce₀.₉Y₀.₁O₂ nanoparticles. On the other hand, the cerium-containing nanoparticles improved electrical properties regardless of the reaction medium. The ASR values of all surface-modified steel samples were below the 0.1 Ω.cm² threshold set for interconnect materials, which was exceeded in the case of the unmodified reference sample. It can be concluded that the applied modifications increased the oxidation resistance of Nirosta 4016/1.4016 to a level that allows its use as SOEC interconnect material. Acknowledgments: Funding of Research project supported by program "Excellence initiative – research university" for the AGH University of Krakow" is gratefully acknowledged (TB).

Keywords: cerium oxide, ferritic stainless steel, gadolinium oxide, interconnect, SOEC

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Authors: Marcos Perez, Christian Dumont, Olivier Nodin, Sebastien Nouveau

Abstract:

Nickel superalloys are used to manufacture high-temperature rotary engine parts such as high-pressure disks in gas turbine engines. High strength at high operating temperatures is required due to the levels of stress and heat the disk must withstand. Therefore it is necessary parts made from materials that can maintain mechanical strength at high temperatures whilst remain comparatively low in cost. A manufacturing process referred to as the triple melt process has made the production of cast and wrought (C&W) nickel superalloys possible. This means that the balance of cost and performance at high temperature may be optimized. AD730TM is a newly developed Ni-based superalloy for turbine disk applications, with reported superior service properties around 700°C when compared to Inconel 718 and several other alloys. The cast ingot is converted into billet during either cogging process or open die forging. The semi-finished billet is then further processed into its final geometry by forging, heat treating, and machining. Conventional ingot-to-billet conversion is an expensive and complex operation, requiring a significant amount of steps to break up the coarse as-cast structure and interdendritic regions. Due to the size of conventional ingots, it is difficult to achieve a uniformly high level of strain for recrystallization, resulting in non-recrystallized regions that retain large unrecrystallized grains. Non-uniform grain distributions will also affect the ultrasonic inspectability response, which is used to find defects in the final component. The main aim is to analyze the recrystallization behavior and microstructural evolution of AD730 at subsolvus temperatures from a semi-finished product (billet) under conditions representative of both cogging and hot forging operations. Special attention to the presence of large unrecrystallized grains was paid. Double truncated cones (DTCs) were hot forged at subsolvus temperatures in hydraulic press, followed by air cooling. SEM and EBSD analysis were conducted in the as-received (billet) and the as-forged conditions. AD730 from billet alloy presents a complex microstructure characterized by a mixture of several constituents. Large unrecrystallized grains present a substructure characterized by large misorientation gradients with the formation of medium to high angle boundaries in their interior, especially close to the grain boundaries, denoting inhomogeneous strain distribution. A fine distribution of intragranular precipitates was found in their interior, playing a key role on strain distribution and subsequent recrystallization behaviour during hot forging. Continuous dynamic recrystallization (CDRX) mechanism was found to be operating in the large unrecrystallized grains, promoting the formation intragranular DRX grains and the gradual recrystallization of these grains. Evidences that hetero-epitaxial recrystallization mechanism is operating in AD730 billet material were found. Coherent γ-shells around primary γ’ precipitates were found. However, no significant contribution to the overall recrystallization during hot forging was found. By contrast, strain presents the strongest effect on the microstructural evolution of AD730, increasing the recrystallization fraction and refining the structure. Regions with low level of deformation (ε ≤ 0.6) were translated into large fractions of unrecrystallized structures (strain accumulation). The presence of undissolved secondary γ’ precipitates (pinning effect), prior to hot forging operations, could explain these results.

Keywords: AD730 alloy, continuous dynamic recrystallization, hot forging, γ’ precipitates

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