Search results for: quarry microstructure

Authors: Aynur Aker, Hasan Kaya

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In recent years, the use of the aluminum based alloys in the industry and technology are increasing. Alloying elements in aluminum have further been improving the strength and stiffness properties that provide superior compared to other metals. In this study, investigation of physical properties (microstructure, microhardness, tensile strength, electrical conductivity and thermal properties) in the Al-12.6wt.%Si-%2wt.Ni ternary alloy were investigated. Al-Si-Ni alloy was prepared in a graphite crucible under vacuum atmosphere. The samples were directionally solidified upwards with different growth rate (V) at constant temperature gradient G (7.73 K/mm). The microstructures (flake spacings, λ), microhardness (HV), ultimate tensile strength, electrical resistivity and thermal properties enthalpy of fusion and specific heat and melting temperature) of the samples were measured. Influence of the growth rate and flake spacings on microhardness, ultimate tensile strength and electrical resistivity were investigated and relationships between them were experimentally obtained by using regression analysis. According to results, λ values decrease with increasing V, but microhardness, ultimate tensile strength, electrical resistivity values increase with increasing V. Variations of electrical resistivity for cast samples with the temperature in the range of 300-1200 K were also measured by using a standard dc four-point probe technique. The enthalpy of fusion and specific heat for the same alloy was also determined by means of differential scanning calorimeter (DSC) from heating trace during the transformation from liquid to solid. The results obtained in this work were compared with the previous similar experimental results obtained for binary and ternary alloys.

Keywords: electrical resistivity, enthalpy, microhardness, solidification, tensile stress

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Authors: M. Riazat, H. Abdolvand, M. Baniassadi

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In this present work, 3D reconstruction of cathode of SOFC is developed with various volume fractions and porosity. Three Phase Boundary (TPB) of construction of such derived micro structures is calculated. The neural network is used to optimize the porosity and volume fraction of each phase to reach a structure with maximum TPB.

Keywords: fuel cell, solid oxide, TPB, 3D reconstruction

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Authors: G. Singh, H.Schuster, U. Füssel

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The stability of electric arc and durability of electrode tip used in Tungsten Inert Gas (TIG) welding demand a metallurgical study about the chemical transport mechanism of emitter oxide particles in tungsten electrode during its real welding conditions. The tungsten electrodes doped with emitter oxides of rare earth oxides such as La₂O₃, Th₂O₃, Y₂O₃, CeO₂ and ZrO₂ feature a comparatively lower work function than tungsten and thus have superior emission characteristics due to lesser surface temperature of the cathode. The local change in concentration of these emitter particles in tungsten electrode due to high temperature diffusion (chemical transport) can change its functional properties like electrode temperature, work function, electron emission, and stability of the electrode tip shape. The resulting increment in tip surface temperature results in the electrode material loss. It was also observed that the tungsten recrystallizes to large grains at high temperature. When the shape of grain boundaries are granular in shape, the intergranular diffusion of oxide emitter particles takes more time to reach the electrode surface. In the experimental work, the microstructure of the used electrode's tip surface will be studied by scanning electron microscope and reflective X-ray technique in order to gauge the extent of the diffusion and chemical reaction of emitter particles. Besides, a simulated model is proposed to explain the effect of oxide particles diffusion on the electrode’s microstructure, electron emission characteristics, and electrode tip erosion. This model suggests metallurgical modifications in tungsten electrode to enhance its erosion resistance.

Keywords: rare-earth emitter particles, temperature-dependent diffusion, TIG welding, Tungsten electrode

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Authors: M. I. Equbal, R. K. Ohdar, B. Singh, P. Talukdar

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Micro-alloyed steel components are used in automotive industry for the necessity to make the manufacturing process cycles shorter when compared to conventional steel by eliminating heat treatment cycles, so an important saving of costs and energy can be reached by reducing the number of operations. Micro-alloying elements like vanadium, niobium or titanium have been added to medium carbon steels to achieve grain refinement with or without precipitation strengthening along with uniform microstructure throughout the matrix. Present study reports the applicability of medium carbon vanadium micro-alloyed steel in hot forging. Forgeability has been determined with respect to different cooling rates, after forging in a hydraulic press at 50% diameter reduction in temperature range of 900-11000C. Final microstructures, hardness, tensile strength, and impact strength have been evaluated. The friction coefficients of different lubricating conditions, viz., graphite in hydraulic oil, graphite in furnace oil, DF 150 (Graphite, Water-Based) die lubricant and dry or without any lubrication were obtained from the ring compression test for the above micro-alloyed steel. Results of ring compression tests indicate that graphite in hydraulic oil lubricant is preferred for free forging and dry lubricant is preferred for die forging operation. Exceptionally good forgeability and high resistance to fracture, especially for faster cooling rate has been observed for fine equiaxed ferrite-pearlite grains, some amount of bainite and fine precipitates of vanadium carbides and carbonitrides. The results indicated that the cooling rate has a remarkable effect on the microstructure and mechanical properties at room temperature.

Keywords: cooling rate, hot forging, micro-alloyed, ring compression

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Authors: Dyah Purwaningsih, Roto Roto, Hari Sutrisno

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Manganese dioxide (MnO₂) and its derivatives are among the most widely used materials for the positive electrode in both primary and rechargeable lithium batteries. The MnO₂ derivative compound of LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) is one of the leading candidates for positive electrode materials in lithium batteries as it is abundant, low cost and environmentally friendly. Over the years, synthesis of LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) has been carried out using various methods including sol-gel, gas condensation, spray pyrolysis, and ceramics. Problems with these various methods persist including high cost (so commercially inapplicable) and must be done at high temperature (environmentally unfriendly). This research aims to: (1) synthesize LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) by reflux technique; (2) develop microstructure analysis method from XRD Powder LiMₓMn₂₋ₓO₄ data with the two-stage method; (3) study the electrical conductivity of LiMₓMn₂₋ₓO₄. This research developed the synthesis of LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) with reflux. The materials consisting of Mn(CH₃COOH)₂. 4H₂O and Na₂S₂O₈ were refluxed for 10 hours at 120°C to form β-MnO₂. The doping of Co, Ni and Cr were carried out using solid-state method with LiOH to form LiMₓMn₂₋ₓO₄. The instruments used included XRD, SEM-EDX, XPS, TEM, SAA, TG/DTA, FTIR, LCR meter and eight-channel battery analyzer. Microstructure analysis of LiMₓMn₂₋ₓO₄ was carried out on XRD powder data by two-stage method using FullProf program integrated into WinPlotR and Oscail Program as well as on binding energy data from XPS. The morphology of LiMₓMn₂₋ₓO₄ was studied with SEM-EDX, TEM, and SAA. The thermal stability test was performed with TG/DTA, the electrical conductivity was studied from the LCR meter data. The specific capacity of LiMₓMn₂₋ₓO₄ as lithium battery cathode was tested using an eight-channel battery analyzer. The results showed that the synthesis of LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) was successfully carried out by reflux. The optimal temperature of calcination is 750°C. XRD characterization shows that LiMn₂O₄ has a cubic crystal structure with Fd3m space group. By using the CheckCell in the WinPlotr, the increase of Li/Mn mole ratio does not result in changes in the LiMn₂O₄ crystal structure. The doping of Co, Ni and Cr on LiMₓMn₂₋ₓO₄ (x = 0.02; 0.04; 0; 0.6; 0.08; 0.10) does not change the cubic crystal structure of Fd3m. All the formed crystals are polycrystals with the size of 100-450 nm. Characterization of LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) microstructure by two-stage method shows the shrinkage of lattice parameter and cell volume. Based on its range of capacitance, the conductivity obtained at LiMₓMn₂₋ₓO₄ (M: Co, Ni, Cr) is an ionic conductivity with varying capacitance. The specific battery capacity at a voltage of 4799.7 mV for LiMn₂O₄; Li₁.₀₈Mn₁.₉₂O₄; LiCo₀.₁Mn₁.₉O₄; LiNi₀.₁Mn₁.₉O₄ and LiCr₀.₁Mn₁.₉O₄ are 88.62 mAh/g; 2.73 mAh/g; 89.39 mAh/g; 85.15 mAh/g; and 1.48 mAh/g respectively.

Keywords: LiMₓMn₂₋ₓO₄, solid-state, reflux, two-stage method, ionic conductivity, specific capacity

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Authors: S. Gupta, R. Sarkar, S. Pathak, D. H. Kela, A. Pramanick, P. Talukdar

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Low alloy quenched and tempered steels are typically used in cast railway components such as knuckles, yokes, and couplers. Since these components experience extensive impact loading during their service life, adequate impact toughness of these grades need to be ensured to avoid catastrophic failure of parts in service. Because of the general availability of Charpy V Test equipment, Charpy test is the most common and economical means to evaluate the impact toughness of materials and is generally used in quality control applications. With this backdrop, an experiment was designed to evaluate the effect of austenitizing temperature, soaking time and resultant grain size on the Charpy impact toughness and the related fracture mechanisms in a quenched and tempered low alloy steel, with the aim of optimizing the heat treatment parameters (i.e. austenitizing temperature and soaking time) with respect to impact toughness. In the first phase, samples were austenitized at different temperatures viz. 760, 800, 840, 880, 920 and 960°C, followed by quenching and tempering at 600°C for 4 hours. In the next phase, samples were subjected to different soaking times (0, 2, 4 and 6 hours) at a fixed austenitizing temperature (980°C), followed by quenching and tempering at 600°C for 4 hours. The samples corresponding to different test conditions were then subjected to instrumented Charpy tests at -40°C and energy absorbed were recorded. Subsequently, microstructure and fracture surface of samples corresponding to different test conditions were observed under scanning electron microscope, and the corresponding grain sizes were measured. In the final stage, austenitizing temperature, soaking time and measured grain sizes were correlated with impact toughness and the fracture morphology and mechanism.

Keywords: heat treatment, grain size, microstructure, retained austenite and impact toughness

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Authors: M.S. El-Feky, Passant Youssef, Mohamed I. Serag

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nowadays, nanotechnology is the main trend of research in different areas due to the new potential of using nanometer materials sized less than 100nm. Nanomaterials are needed in cement composites to act as bridging for Nano and micro-cracks to increase tensile strength, reduce the permeability of gases and water in concrete to solve corrosion problem, react with excess Calcium Hydroxide, produce additional C-S-H, act as filler materials to densify the cement matrix and increase its mechanical properties. The present study focuses on the effectiveness of super-plasticizers and ultrasonic processing on the dispersion of Carbon Nanotube at first in water and then in cement composites in combination with Nano silica to enhance the mechanical properties of cement composites. A qualitative analysis using a compressive strength test is conducted with a view to investigate the influence of different dispersion techniques on the mechanical properties of cement composites containing Carbon Nanotube (CNT) and Nano Silica (NS) particles with different percentages. In addition, micro-structural analysis was carried out to understand the surface morphology and microstructure of cement composites with different dosages of NS addition. The investigational study results showed that the combination of NS with a low amount of CNT had a positive effect on the hydration reaction; on the other hand, the combination of CNT and a high amount of NS had a negative effect on the hydration reaction. The compressive strength can be improved by optimum combination 0.02% CNT and 1% NS with gain in strength by 72% and 35% after 7 and 28 days compared to control samples; these results were with an agreement with the morphology structure of composites using microstructure analysis.

Keywords: nano silica, dispersion, sonication, carbon nano tubes

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Authors: Samiha Ramdani, Abdelhamid Geuttala

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There is no doubt that the batteries increasingly used tires create environmental concerns. Algeria generates large amounts of by industrial and household waste, such as used tires and colored glass bottles and dishes, whose valuation in cementitious materials could be an interesting ecological and economical alternative for broadening eliminating cumbersome landfills. This work is a contribution to the promotion of local materials with the use of waste tires and glass bottle in the development of a new cementitious composite having the acceptable compressive strength and a capacity of improved strains. For this purpose, rubber crumb (GC) from shredding used tires were used as partial replacement of quarry sand with 10%, 20%, 40, 60%. In addition, some mixtures also contain glass powder at15% cement replacement by volume. The compressive strength, tensile strength, deformability, the water permeability and penetration Inions chlorides are studied. As results; an acceptable compressive strength was obtained with the substitution rate of 10% and 20% by volume, the deformability of the composite increases with increased replacement rate. The addition of finely ground glass as a partial replacement of cement concrete increases the resistance to penetration of Inions chloride and reduce the water permeability thereof; then increases their durability.

Keywords: crumb rubber, deformability, compressive strength, finely ground glass, durability, behavior law

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Authors: Deepa T., Inchara S. R., Venkatesh S. V., Seema Tharannum

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Concrete is the most widely used structural material. It is usually made using locally available materials. However, concrete has low tensile strength and may crack in the early days with exothermic hydration, for which water is essential. To address the increased construction water demand, treated greywater may be used. Bacillus subtilis bacteria that form endospores is the biological agent considered in this study for biomineralization or Microbially Induced Calcite Precipitation (MICP) technique to heal cracks. Treated grey water which is obtained from STP of PES University, opted in place of Potable water, which had qualities within the standard range as per codal provisions. In this work, M30 grade conventional concrete is designed using OPC 53-grade cement, manufactured sand, natural coarse aggregates, and potable water. Conventional concrete (CC), bacterial concrete with potable water (BS), and treated grey water concrete (TGWBS) are the three different concrete specimens cast. Experimental studies such as the strength test and the surface hardness test are performed on conventional and bacterial concrete samples after 7, 28, and 56 days of curing. Concrete cubes are subjected to a temperature of 50° C to investigate the effect of higher temperature. Cracked cube specimens are observed for self-healing -as well as microstructure analysis with Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Analysis (EDAX), and X-Ray Diffraction Analysis (XRD). Noticeable calcium salt deposition is observed on the surface of the BS and TGWBS cracked specimen. Surface hardness and the EDAX test gave promising results on the advantage of using spore-forming bacteria in concrete. This is followed by the strength gained in compression and flexure. Results also indicate that treated grey water can be a substitute for potable water in concrete.

Keywords: Bacillus subtilis concrete, microstructure, temperature, treated greywater

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Authors: M. N. Baig, F. N. Khan, M. Junaid

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Titanium alloys are widely employed in aerospace, medical, chemical, and marine applications. These alloys offer many advantages such as low specific weight, high strength to weight ratio, excellent corrosion resistance, high melting point and good fatigue behavior. These attractive properties make titanium alloys very unique and therefore they require special attention in all areas of processing, especially welding. In this work, 1.6 mm thick sheets of Ti-5Al-2,5Sn, an alpha titanium (α-Ti) alloy, were welded using electron beam (EBW) and laser beam (LBW) welding processes to achieve a full penetration Bead-on Plate (BoP) configuration. The weldments were studied using polarized optical microscope, SEM, EDS and XRD. Microhardness distribution across the weld zone and smooth and notch tensile strengths of the weldments were also recorded. Residual stresses using Hole-drill Strain Measurement (HDSM) method and deformation patterns of the weldments were measured for the purpose of comparison of the two welding processes. Fusion zone widths of both EBW and LBW weldments were found to be approximately equivalent owing to fairly similar high power densities of both the processes. Relatively less oxide content and consequently high joint quality were achieved in EBW weldment as compared to LBW due to vacuum environment and absence of any shielding gas. However, an increase in heat-affected zone width and partial ά-martensitic transformation infusion zone of EBW weldment were observed because of lesser cooling rates associated with EBW as compared with LBW. The microstructure infusion zone of EBW weldment comprised both acicular α and ά martensite within the prior β grains whereas complete ά martensitic transformation was observed within the fusion zone of LBW weldment. Hardness of the fusion zone in EBW weldment was found to be lower than the fusion zone of LBW weldment due to the observed microstructural differences. Notch tensile specimen of LBW exhibited higher load capacity, ductility, and absorbed energy as compared with EBW specimen due to the presence of high strength ά martensitic phase. It was observed that the sheet deformation and deformation angle in EBW weldment were more than LBW weldment due to relatively more heat retention in EBW which led to more thermal strains and hence higher deformations and deformation angle. The lowest residual stresses were found in LBW weldments which were tensile in nature. This was owing to high power density and higher cooling rates associated with LBW process. EBW weldment exhibited highest compressive residual stresses due to which the service life of EBW weldment is expected to improve.

Keywords: Laser and electron beam welding, Microstructure and mechanical properties, Residual stress and distortions, Titanium alloys

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Authors: Yonosuke Murayama

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We have developed and studied a metastable beta Ti alloy, which shows super-elasticity and low Young’s modulus according to the phase stability of its beta phase. The super-elasticity and low Young’s modulus are required in a wide range of applications in various industrial fields. For example, the metallic implant with low Young’s modulus and non-toxicity is desirable because the large difference of Young’s modulus between the human bone and the implant material may cause a stress-shielding phenomenon. We have investigated the role of Sn and Al in metastable beta Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys. The metastable beta Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys form during quenching from the beta field at high temperature. While Cr and V act as beta stabilizers, Sn and Al are considered as elements to suppress the athermal omega phase produced during quenching. The athermal omega phase degrades the properties of super-elasticity and Young’s modulus. Although Al and Sn as single elements are considered as an alpha stabilizer and neutral, respectively, Sn and Al acted also as beta stabilizers when added simultaneously with beta stabilized element of Cr or V in this experiment. The quenched microstructure of Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys shifts from martensitic structure to beta single-phase structure with increasing Cr or V. The Young’s modulus of Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys decreased and then increased with increasing Cr or V, each showing its own minimum value of Young's modulus respectively. The composition of the alloy with the minimum Young’s modulus is a near border composition where the quenched microstructure shifts from martensite to beta. The border composition of Ti-Cr-Sn and Ti-V-Sn alloys required only less amount of each beta stabilizer, Cr or V, than Ti-Cr-Al and Ti-V-Al alloys. This indicates that the effect of Sn as a beta stabilizer is stronger than Al. Sn and Al influenced the competitive relation between stress-induced martensitic transformation and slip deformation. Thus, super-elastic properties of metastable beta Ti-Cr-Sn, Ti-Cr-Al, Ti-V-Sn, and Ti-V-Al alloys varied depending on the alloyed element, Sn or Al.

Keywords: metastable beta Ti alloy, super-elasticity, low Young’s modulus, stress-induced martensitic transformation, beta stabilized element

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Authors: Ifeyinwa Ijeoma Obianyo, Luqman Adedeji Taiwo, Olugbenga O. Amu, Azikiwe Peter Onwualu

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Improving the durability of building materials saves maintenance costs, construction time, and energy. In this study, titanium dioxide coated conventional and non-conventional composites were produced, and the effects of titanium dioxide coatings were investigated. Conventional composites were produced using river sand and Portland cement, whereas non-conventional composites were produced by partially replacing river sand and Portland cement with quarry dust and rice husk ash. Water absorption and thickness swelling tests were conducted on the produced coated and non-coated block samples. A reduction in water absorption was observed in the coated composite samples when compared to the non-coated composite samples, and this is an indication of the improved durability of the samples coated with titanium dioxide. However, there was an increase in the thickness swelling of coatings on the coated block samples, but this increase has a slight influence on the compressive strength of the coated samples. The outcome of this study indicates that coating composite building blocks with titanium dioxide will improve theirdurability. Also, the site exposure experiments revealed the self-cleansing properties of TiO2-coated composite block samples, while the Rhodamine B discolouration test confirmed the photocatalytic features of TiO2-coated composite block samples.

Keywords: titanium dioxide, water absorption, durability, mechanical properties, building composite

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Authors: Jae-Ho Jang, Jung-Soo Kim, Byung-Jun Kim, Dae-Geun Nam, Uoo-Chang Jung, Yoon-Suk Choi

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Low alloy steels are widely used for pressure vessels, spent fuel storage, and steam generators required to withstand the internal pressure and prevent unexpected failure in nuclear power plants, which these may suffer embrittlement by high levels of radiation and heat for a long period. Therefore, it is important to improve mechanical properties of low alloy steels for the integrity of structure materials at an early stage of fabrication. Recently, it showed that a double austenitizing and tempering (DTA) process resulted in a significant improvement of strength and toughness by refinement of prior austenite grains. In this study, it was investigated that the mechanism of improving mechanical properties according to the change of microstructure by the second fully austenitizing temperature of the DAT process for low alloy steel required the structural integrity. Compared to conventional single austenitizing and tempering (SAT) process, the tensile elongation properties have improved about 5%, DBTTs have obtained result in reduction of about -65℃, and grain size has decreased by about 50% in the DAT process conditions. Grain refinement has crack propagation interference effect due to an increase of the grain boundaries and amount of energy absorption at low temperatures. The higher first austenitizing temperature in the DAT process, the more increase the spheroidized carbides and strengthening the effect of fine precipitates in the ferrite grain. The area ratio of the dimple in the transition area has increased by proportion to the effect of spheroidized carbides. This may the primary mechanisms that can improve low-temperature toughness and elongation while maintaining a similar hardness and strength.

Keywords: double austenitizing, Ductile Brittle transition temperature, grain refinement, heat treatment, low alloy steel, low-temperature toughness

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Authors: Longkui Zhu, Zhengcao Li

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High temperature gas-cooled reactors (HTGRs) are considered as one of the next-generation advanced nuclear reactors, in which porous nuclear graphite is used as neutron moderators, reflectors, structure materials, and cooled by inert helium. Radioactive tritium and ¹⁴C are generated in terms of reactions of thermal neutrons and ⁶Li, ¹⁴N, ¹⁰B impurely within nuclear graphite and the coolant during HTGRs operation. Currently, hydrogen and nitrogen diffusion behavior together with nuclear graphite microstructure evolution were investigated to minimize the radioactive waste release, using thermogravimetric analysis, X-ray computed tomography, the BET and mercury standard porosimetry methods. It is found that the peak value of graphite weight loss emerged at 573-673 K owing to nitrogen diffusion from graphite pores to outside when the system was subjected to vacuum. Macropore volume became larger while porosity for mesopores was smaller with temperature ranging from ambient temperature to 1073 K, which was primarily induced by coalescence of the subscale pores. It is suggested that the porous nuclear graphite should be first subjected to vacuum at 573-673 K to minimize the nitrogen and the radioactive 14°C before operation in HTGRs. Then, results on hydrogen diffusion show that the diffusible hydrogen and tritium could permeate into the coolant with diffusion coefficients of > 0.5 × 10⁻⁴ cm²·s⁻¹ at 50 bar. As a consequence, the freshly-generated diffusible tritium could release quickly to outside once formed, and an effective approach for minimizing the amount of radioactive tritium is to make the impurity contents extremely low in nuclear graphite and the coolant. Besides, both two- and three-dimensional observations indicate that macro and mesopore volume along with total porosity decreased with temperature at 50 bar on account of synergistic effects of applied compression strain, sharpened pore morphology, and non-uniform temperature distribution.

Keywords: advanced high temperature gas-cooled reactor, hydrogen and nitrogen diffusion, microstructure evolution, nuclear graphite, radioactive waste management

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Authors: Bing–Jing Zhao, Chang-Kui Liu, Hong Wang, Min Hu

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Electron beam rapid manufacturing (EBRM) or Selective laser melting is an additive manufacturing process that uses 3D CAD data as a digital information source and energy in the form of a high-power laser beam or electron beam to create three-dimensional metal parts by fusing fine metallic powders together.Object:The present study was conducted to evaluate the mechanical properties ,the phase transformation,the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM,SLM and forging technique.Method: Ti-6Al-4V alloy standard test pieces were manufactured by EBRM, SLM and forging technique according to AMS4999,GB/T228 and ISO 10993.The mechanical properties were analyzed by universal test machine. The phase transformation was analyzed by X-ray diffraction and scanning electron microscopy. The corrosivity was analyzed by electrochemical method. The biocompatibility was analyzed by co-culturing with mesenchymal stem cell and analyzed by scanning electron microscopy (SEM) and alkaline phosphatase assay (ALP) to evaluate cell adhesion and differentiation, respectively. Results: The mechanical properties, the phase transformation, the corrosivity and the biocompatibility of Ti-6Al-4V by EBRM、SLM were similar to forging and meet the mechanical property requirements of AMS4999 standard. a­phase microstructure for the EBM production contrast to the a’­phase microstructure of the SLM product. Mesenchymal stem cell adhesion and differentiation were well. Conclusion: The property of the Ti-6Al-4V alloy manufactured by EBRM and SLM technique can meet the medical standard from this study. But some further study should be proceeded in order to applying well in clinical practice.

Keywords: 3D printing, Electron Beam Rapid Manufacturing (EBRM), Selective Laser Melting (SLM), Computer Aided Design (CAD)

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Authors: Yebeen Ji, Jimin Yun, Kwonhoo Kim

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Magnesium alloys were limited for industrial applications due to having a limited slip system and high plastic anisotropy. It has been known that specific textures were formed during processing (rolling, etc.), and These textures cause poor formability. To solve these problems, many researchers have studied controlling texture by adding rare-earth elements. However, the high cost limits their use; therefore, alternatives are needed to replace them. Although Pb addition doesn’t directly improve magnesium properties, it has been known to suppress the diffusion of other alloying elements and reduce grain boundary energy. These characteristics are similar to the additions of rare-earth elements, and a similar texture behavior is expected as well. However, there is insufficient research on this. Therefore, this study investigates the behavior of texture and microstructure development after adding Pb to magnesium. This study compared and analyzed AZ61 alloy and Mg-15wt%Pb alloy to determine the effect of adding solute elements. The alloy was hot rolled and annealed to form a single phase and initial texture. Afterward, the specimen was set to contraction and elongate parallel to the rolling surface and the rolling direction and then subjected to high-temperature plane strain compression under the conditions of 723K and 0.05/s. Microstructural analysis and texture measurements were performed by SEM-EBSD. The peak stress in the true strain-stress curve after compression was higher in AZ61, but the shape of the flow curve was similar for both alloys. For both alloys, continuous dynamic recrystallization was confirmed to occur during the compression process. The basal texture developed parallel to the compressed surface, and the pole density was lower in the Mg-15wt%Pb alloy. It is confirmed that this change in behavior is because the orientation distribution of recrystallized grains has a more random orientation compared to the parent grains when Pb is added.

Keywords: Mg, texture, Pb, DRX

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Authors: L. Gyansah, Yanfang Shen, Jiqiang Wang, Tianying Xiong

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SiCₚ/ pure Al composites with different SiC fractions (20 wt %, 30 wt %, and 40 wt %) were precisely cold sprayed, followed by hot axial-compression tests at deformation temperatures of 473 K to 673 K, leading to failure of specimens through routine crack propagation in their multiphase. The plastic deformation behaviour with respect to the SiCₚ contents and the deformation temperatures were studied at strain rate 1s-1.As-sprayed and post-failure specimens were analyzed by X-ray computed tomography (XCT), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Quasi-static thermomechanical testing results revealed that compressive strength (UTS = 228 MPa and 30.4 %) was the highest in the composites that was thermomechanically compressed at 473 K compared to those of the as-sprayed, while the as-sprayed exhibited a compressive strength of 182.8 MPa related to the increment in SiC fraction. Strength—plasticity synergy was promoted by dynamic recrystallization (DRX) through strengthening and refinement of the grains. The DRX degree depends relevantly on retainment of the uniformly ultrafine SiCₚ particulates, the pinning effects of the interfaces promoted by the ultrafine grain structures (UFG), and the higher deformation temperature. Reconstructed X-ray computed tomography data revealed different crack propagation mechanisms. A single-plane shear crack with multi-laminates fracture morphology yields relatively through the as-sprayed and as-deformed at 473 K deposits, while a multiphase plane shear cracks preeminently existed in high temperature deformed deposits resulting in multiphase-interface delaminations. Three pertinent strengthening mechanisms, videlicet, SiCp dispersed strengthening, refined grain strengthening, and dislocation strengthening, existed in the gradient microstructure, and their detailed contributions to the thermomechanical properties were discussed.

Keywords: cold spraying, hot deformation, deformation temperature, thermomechancal properties, SiC/Al composite

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Authors: Zue Chin Chang, Shih-Chang Liang

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RF magnetron sputtering is used on the ceramic targets, each of which contains zinc oxide (ZnO), zinc oxide doped with aluminum (AZO) and zinc oxide doped with gallium (GZO). The electric conduction mechanism of the AZO and GZO films came mainly from the Al and Ga, the oxygen vacancies, Zn interstitial atoms, and Al and/or Ga interstitial atoms. AZO and GZO films achieved higher conduction than did ZnO film, it being ion vacant and nonstoichiometric. The XRD analysis showed a preferred orientation along the (002) plane for ZnO, AZO, and GZO films.

Keywords: ZnO, AZO, GZO, doped, sputtering

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Authors: Sandrine Cardinal, Jean-Marc Pelletier, Guang Xie, Florian Mercier, Florent Delmas

Abstract:

Bulk metallic glasses exhibit several superior properties, compared to their corresponding crystalline counterpart, such as high strength, high elastic limit or good corrosion resistance. Therefore they can be considered as good candidates for structural applications in many sectors. However, they are generally brittle and do not exhibit plastic deformation at room temperature. These materials are mainly obtained by rapid cooling from a liquid state to prevent crystallization, which limits their size. To overcome these two drawbacks: fragility and limited dimensions, composite metallic glass matrix reinforced by a second phase whose role is to slow crack growth are developed. Concerning the limited size of the pieces, the proposed solution is to get the material from amorphous powders by densifying under load. In this study, Cu50Zr45Al5 bulk metallic glassy matrix composites (MGMCs) containing different volume fraction (Vf) of Zr crystalline particles were manufactured by spark plasma sintering (SPS). Microstructure, thermal stability and mechanical properties of the MGMCs were investigated. Matrix of the composites remains a fully amorphous phase after consolidation at 420°C under 600 MPa. A good dispersion of the particles in the glassy matrix is obtained. Results show that the compressive strength decreases with Vf : 1670 MPa (Vf=0%) to 1300MPa (Vf=30%), the elastic modulus decreases but only slighty respectively 97.3GPa and 94.5 GPa and plasticity is improved from 0 to 4%. Fractographic investigation indicates a good bonding between amorphous and crystalline particles. In conclusion, present study has demonstrated that SPS method is useful for the synthesis of the bulk glassy composites. Large controlled microstructure specimens with interesting ductility can be obtained compared with others methods.

Keywords: composite, mechanical properties, metallic glasses, spark plasma sintering

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Authors: Blanca A. Pichardo, Victor H. Lopez, Melchor Salazar, Rafael Garcia, Alberto Ruiz

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Clad pipes in comparison to plain carbon steel pipes offer the oil and gas industry high corrosion resistance, reduction in economic losses due to pipeline failures and maintenance, lower labor risk, prevent pollution and environmental damage due to hydrocarbons spills caused by deteriorated pipelines. In this context, it is paramount to establish reliable welding procedures to join bimetallic plates or pipes. Thus, the aim of this work is to study the microstructure and mechanical behavior of clad plates welded by the gas metal arc welding (GMAW) process. A clad of 316L stainless steel was deposited onto API 5L X-60 plates by overlay welding with the GMAW process. Welding parameters were, 22.5 V, 271 A, heat input 1,25 kJ/mm, shielding gas 98% Ar + 2% O₂, reverse polarity, torch displacement speed 3.6 mm/s, feed rate 120 mm/s, electrode diameter 1.2 mm and application of an electromagnetic field of 3.5 mT. The overlay welds were subjected to macro-structural and microstructural characterization. After manufacturing the clad plates, a single V groove joint was machined with a 60° bevel and 1 mm root face. GMA welding of the bimetallic plates was performed in four passes with ER316L-Si filler for the root pass and an ER70s-6 electrode for the subsequent welding passes. For joining the clad plates, an electromagnetic field was applied with 2 purposes; to improve the microstructural characteristics and to assist the stability of the electric arc during welding in order to avoid magnetic arc blow. The welds were macro and microstructurally characterized and the mechanical properties were also evaluated. Vickers microhardness (100 g load for 10 s) measurements were made across the welded joints at three levels. The first profile, at the 316L stainless steel cladding, was quite even with a value of approximately 230 HV. The second microhardness profile showed high values in the weld metal, ~400 HV, this was due to the formation of a martensitic microstructure by dilution of the first welding pass with the second. The third profile crossed the third and fourth welding passes and an average value of 240 HV was measured. In the tensile tests, yield strength was between 400 to 450 MPa with a tensile strength of ~512 MPa. In the Charpy impact tests, the results were 86 and 96 J for specimens with the notch in the face and in the root of the weld bead, respectively. The results of the mechanical properties were in the range of the API 5L X-60 base material. The overlap welding process used for cladding is not suitable for large components, however, it guarantees a metallurgical bond, unlike the most commonly used processes such as thermal expansion. For welding bimetallic plates, control of the temperature gradients is key to avoid distortions. Besides, the dissimilar nature of the bimetallic plates gives rise to the formation of a martensitic microstructure during welding.

Keywords: clad pipe, dissimilar welding, gas metal arc welding, magnetic fields

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Authors: Shahril Anuar Bahari, Mohd Azrie Mohd Kepli, Mohd Ariff Jamaludin, Kamarulzaman Nordin, Mohamad Jani Saad

Abstract:

Formaldehyde release from wood-based panel composites can be very toxicity and may increase the risk of human health as well as environmental problems. A new bio-composites product without synthetic adhesive or resin is possible to be developed in order to reduce these problems. Apart from formaldehyde release, adhesive is also considered to be expensive, especially in the manufacturing of composite products. Natural bonded composites can be termed as a panel product composed with any type of cellulosic materials without the addition of synthetic resins. It is composed with chemical content activation in the cellulosic materials. Pulp and paper making method (chemical pulping) was used as a general guide in the composites manufacturing. This method will also generally reduce the manufacturing cost and the risk of formaldehyde emission and has potential to be used as an alternative technology in fiber composites industries. In this study, the natural bonded bamboo fiber composite was produced from virgin Malaysian bamboo fiber (Bambusa vulgaris). The bamboo culms were chipped and digested into fiber using this pulping method. The black liquor collected from the pulping process was used as a natural binding agent in the composition. Then the fibers were mixed and blended with black liquor without any resin addition. The amount of black liquor used per composite board was 20%, with approximately 37% solid content. The composites were fabricated using a hot press machine at two different board densities, 850 and 950 kg/m³, with two sets of hot pressing time, 25 and 35 minutes. Samples of the composites from different densities and hot pressing times were tested in flexural strength and internal bonding (IB) for strength performance according to British Standard. Modulus of elasticity (MOE) and modulus of rupture (MOR) was determined in flexural test, while tensile force perpendicular to the surface was recorded in IB test. Results show that the strength performance of the composites with 850 kg/m³ density were significantly higher than 950 kg/m³ density, especially for samples from 25 minutes hot pressing time. Strength performance of composites from 25 minutes hot pressing time were generally greater than 35 minutes. Results show that the maximum mean values of strength performance were recorded from composites with 850 kg/m³ density and 25 minutes pressing time. The maximum mean values for MOE, MOR and IB were 3251.84, 16.88 and 0.27 MPa, respectively. Only MOE result has conformed to high density fiberboard (HDF) standard (2700 MPa) in British Standard for Fiberboard Specification, BS EN 622-5: 2006. Microstructure characteristics of composites can also be related to the strength performance of the composites, in which, the observed fiber damage in composites from 950 kg/m³ density and overheat of black liquor led to the low strength properties, especially in IB test.

Keywords: bamboo fiber, natural bonded, black liquor, mechanical tests, microstructure observations

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Authors: Mario Alejandro Grisales, M. Daniela Chimá, Gilberto Bejarano Gaitán

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High entropy alloys (HEA) and nitride (HEN) are currently very attractive to the automotive, aerospace, metalworking and materials forming manufacturing industry, among others, for exhibiting higher mechanical properties, wear resistance, and thermal stability than binary and ternary alloys. In this work medium-entropy coatings of TiTaZrNb and the nitrides of (TiTaZrNb)Nx were synthesized on to AISI 420 and M2 steel samples by the direct current magnetron sputtering technique. The influence of the bias voltage supplied to the substrate on the microstructure, chemical- and phase composition of the matrix coating was evaluated, and the effect of nitrogen flow on the microstructural, mechanical and tribological properties of the corresponding nitrides was studied. A change in the crystalline structure from BCC for TiTaZrNb coatings to FCC for (TiTaZrNb)Nx was observed, that is associated with the incorporation of nitrogen into the matrix and the consequent formation of a solid solution of (TiTaZrNb)Nx. An increase in hardness and residual stresses was observed with increasing bias voltage for TiTaZrNb, reaching 12.8 GPa for the coating deposited with a bias of -130V. In the case of (TiTaZrNb)Nx nitride, a greater hardness of 23 GPa is achieved for the coating deposited with a N2 flow of 12 sccm, which slightly drops to 21.7 GPa for that deposited with N2 flow of 15 sccm. The slight reduction in hardness could be associated with the precipitation of the TiN and ZrN phases that are formed at higher nitrogen flows. The specific wear rate of the deposited coatings ranged between 0.5xexp13 and 0.6xexp13 N/m2. The steel substrate exhibited an average hardness of 2.0 GPa and a specific wear rate of 203.2exp13 N/m2. Both the hardness and the specific wear rate of the synthesized nitride coatings were higher than that of the steel substrate, showing a protective effect of the steel against wear.

Keywords: medium entropy coatings, hard coatings, magnetron sputtering, tribology, wear resistance

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Authors: Devender Sharma, Shweta Goyal

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Sustainable development is a key to protect the environment for a secure future. Accelerated carbonation curing is a comparatively new technique for curing of concrete which involves sequestration of carbon dioxide gas into the precast concrete, resulting in improvement of the properties of concrete. This paper presents the results of a study to evaluate the effect of carbonation curing on cement mortars incorporating cement kiln dust (CKD) as partial replacement of cement. The mortar specimens were prepared by replacing cement with CKD in varying percentages of 0-50% by the weight of cement. The specimens were subjected to 12 hour carbonation curing, followed by sealed packing till testing age. The results were compared with the normal curing procedure, in which the specimens were water cured till the testing age. Compressive strength and microstructure of the mix were studied. It was noted that on increasing the percentage of CKD up to 10% by the weight of the cement, no considerable change was observed in the compressive strength. But as the percentage of CKD was further increased, there was a decrease in compressive strength, with strength decreasing up to 40% when 50% of the cement was replaced with CKD. The decrease in strength is due to the lesser lime content in CKD as compared to cement. High ettringite formation was observed in mixes with high percentages of CKD, thus indicating a decrease in the compressive strength. With carbonation curing, an early age strength gain was observed in mortars, even with higher percentages of CKD. The early strength of the carbonation cured mixes was found to be greater than water cured mixes irrespective of the percentage of CKD. 7 days and 28 days compressive strength of the mix was comparable for both the carbonation cured and water cured specimen. The increase in compressive strength can be attributed to the conversion of unstable Ca(OH)2 into stable CaCO3, which causes densification of the mix. CaCO3 precipitation and greater CSH gel formation was clearly observed in the SEM images of carbonation cured specimen, indicating higher compressive strength. Thus, carbonation curing can be used as an efficient method to enhance the properties of concrete.

Keywords: carbonation, cement kiln dust, compressive strength, microstructure

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Authors: B. J. Babalola, M. B. Shongwe

Abstract:

Spark Plasma Sintering technique is a novel processing method that produces limited grain growth and highly dense variety of materials; alloys, superalloys, and carbides just to mention a few. However, initial particle size and spark plasma sintering parameters are factors which influence the grain growth and mechanical properties of sintered materials. Ni-Cr alloys are regarded as the most promising alloys for aerospace turbine blades, owing to the fact that they meet the basic requirements of desirable mechanical strength at high temperatures and good resistance to oxidation. The conventional method of producing this alloy often results in excessive grain growth and porosity levels that are detrimental to its mechanical properties. The effect of sintering temperature was evaluated on the microstructure and mechanical properties of the nanostructured Ni-17Cr alloy. Nickel and chromium powder were milled using high energy ball milling independently for 30 hours, milling speed of 400 revs/min and ball to powder ratio (BPR) of 10:1. The milled powders were mixed in the composition of Nickel having 83 wt % and chromium, 17 wt %. This was sintered at varied temperatures from 800°C, 900°C, 1000°C, 1100°C and 1200°C. The structural characteristics such as porosity, grain size, fracture surface and hardness were analyzed by scan electron microscopy and X-ray diffraction, Archimedes densitometry, micro-hardness tester. The corresponding results indicated an increase in the densification and hardness property of the alloy as the temperature increases. The residual porosity of the alloy reduces with respect to the sintering temperature and in contrast, the grain size was enhanced. The study of the mechanical properties, including hardness, densification shows that optimum properties were obtained for the sintering temperature of 1100°C. The advantages of high sinterability of Ni-17Cr alloy using milled powders and microstructural details were discussed.

Keywords: densification, grain growth, milling, nanostructured materials, sintering temperature

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Authors: S. Ziaran, M. Musil, M. Cekan, O. Chlebo

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The paper analyzes the response of buildings and industrially structures on seismic waves (low frequency mechanical vibration) generated by blasting operations. The principles of seismic analysis can be applied for different kinds of excitation such as: earthquakes, wind, explosions, random excitation from local transportation, periodic excitation from large rotating and/or machines with reciprocating motion, metal forming processes such as forging, shearing and stamping, chemical reactions, construction and earth moving work, and other strong deterministic and random energy sources caused by human activities. The article deals with the response of seismic, low frequency, mechanical vibrations generated by nearby blasting operations on a residential home. The goal was to determine the fundamental natural frequencies of the measured structure; therefore it is important to determine the resonant frequencies to design a suitable modal damping. The article also analyzes the package of seismic waves generated by blasting (Primary waves – P-waves and Secondary waves S-waves) and investigated the transfer regions. For the detection of seismic waves resulting from an explosion, the Fast Fourier Transform (FFT) and modal analysis, in the frequency domain, is used and the signal was acquired and analyzed also in the time domain. In the conclusions the measured results of seismic waves caused by blasting in a nearby quarry and its effect on a nearby structure (house) is analyzed. The response on the house, including the fundamental natural frequency and possible fatigue damage is also assessed.

Keywords: building structure, seismic waves, spectral analysis, structural response

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Authors: D. T. Chabalala, J. M. Ndambuki, M. F. Ilunga

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Sedimentation includes the processes of erosion, transportation, deposition, and the compaction of sediment. Sedimentation in reservoir results in a decrease in water storage capacity, downstream problems involving aggregation and degradation, blockage of the intake, and change in water quality. A study was conducted in Caledon River catchment in the upstream of Welbedacht Reservoir located in the South Eastern part of Free State province, South Africa. The aim of this research was to investigate and develop a model for an Integrated Catchment Modelling of Sedimentation processes and management for the Welbedacht reservoir. Revised Universal Soil Loss Equation (RUSLE) was applied to determine sources of sediment at different areas of the catchment. The model has been also used to determine the impact of changes from management practice on erosion generation. The results revealed that the main sources of sediment in the watershed are cultivated land (273 ton per hectare), built up and forest (103.3 ton per hectare), and grassland, degraded land, mining and quarry (3.9, 9.8 and 5.3 ton per hectare) respectively. After application of soil conservation practices to developed Revised Universal Soil Loss Equation model, the results revealed that the total average annual soil loss in the catchment decreased by 76% and sediment yield from cultivated land decreased by 75%, while the built up and forest area decreased by 42% and 99% respectively. Thus, results of this study will be used by government departments in order to develop sustainable policies.

Keywords: Welbedacht reservoir, sedimentation, RUSLE, Caledon River

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Authors: Jie Ren, Siyao Guo

Abstract:

Laden with phosphates at a low pH value, sewage wastewater aggressive environments constitute a great threat to concrete-based pipes which is made of alkaline cementitious materials such as ordinary Portland cement (OPC). As a promising alternative for OPC-based binders, alkali-activated slag/fly ash (AASF) cementitious binders are generally believed to gain similar or better properties compared to OPC-based counterparts, especially durability. However, there is limited research on the performance of AASF binders in phosphoric acid solution. Moreover, the behavior of AASF binders composited with epoxy resin/TiO₂ when exposed to acidic media has been rarely explored. In this study, the performance of AASF paste with the precursor slag:fly ash (50:50 in mass ratio) enhanced with epoxy resin/TiO₂ composite in phosphoric acid solution (pH = 3.0-4.0) was investigated. The exposure towards acid attack lasted for 90 days. The same AASF mixture without resin/TiO₂ composite was used as a reference. The compressive strength and porous-related properties prior to acidic immersion were tested. The mass variations and degradation depth of the two mixtures of binders were also monitored which is based on phenolphthalein-videomicroscope method. The results show that the binder with epoxy resin/TiO₂ addition gained a higher compressive strength and lower water absorption than the reference. In addition, it also displayed a higher resistance towards acid attack indicated by a less mass loss and less degradation depth compared to the control sample. This improvement can be attributed to a dense microstructure evidenced by the higher compressive strength and related porous structures. It can be concluded that the microstructure can be improved by adding epoxy resin/TiO₂ composite in order to enhance the resistance of AASF binder towards acid attacks.

Keywords: alkali-activated paste, epoxy resin/TiO₂, composites, mechanical properties, phosphoric acid

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Authors: M. S. Nandana, K. Udaya Bhat, C. M. Manjunatha

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In this study aluminum alloy 7010 was subjected to three different ageing treatments i.e., peak ageing (T6), over-ageing (T7451) and retrogression and re ageing (RRA) to study the influence of precipitate microstructure on the fatigue crack growth rate behavior. The microstructural modification was studied by using transmission electron microscope (TEM) to examine the change in the size and morphology of precipitates in the matrix and on the grain boundaries. The standard compact tension (CT) specimens were fabricated and tested under constant amplitude fatigue crack growth tests to evaluate the influence of heat treatment on the fatigue crack growth rate properties. The tests were performed in a computer-controlled servo-hydraulic test machine applying a load ratio, R = 0.1 at a loading frequency of 10 Hz as per ASTM E647. The fatigue crack growth was measured by adopting compliance technique using a CMOD gauge attached to the CT specimen. The average size of the matrix precipitates were found to be of 16-20 nm in T7451, 5-6 nm in RRA and 2-3 nm in T6 conditions respectively. The grain boundary precipitate which was continuous in T6, was disintegrated in RRA and T7451 condition. The PFZ width was lower in RRA compared to T7451 condition. The crack growth rate was higher in T7451 and lowest in RRA treated alloy. The RRA treated alloy also exhibits an increase in threshold stress intensity factor range (∆Kₜₕ). The ∆Kₜₕ measured was 11.1, 10.3 and 5.7 MPam¹/² in RRA, T6 and T7451 alloys respectively. The fatigue crack growth rate in RRA treated alloy was nearly 2-3 times lower than that in T6 and was one order lower than that observed in T7451 condition. The surface roughness of RRA treated alloy was more pronounced when compared to the other conditions. The reduction in fatigue crack growth rate in RRA alloy was majorly due to the increase in roughness and partially due to increase in spacing between the matrix precipitates. The reduction in crack growth rate and increase in threshold stress intensity range is expected to benefit the damage tolerant capability of aircraft structural components under service loads.

Keywords: damage tolerance, fatigue, heat treatment, PFZ, RRA

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Authors: C. Nakib, N. Ammouchi, A. Otmani, A. Djekoun, J. M. Grenèche

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B2-structured FeAl was synthesized by an abrupt reaction during mechanical alloying (MA) of the elemental powders of Fe, Al and Ni. The structural, microstructural and morphological changes occurring in the studied material during MA were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Two crystalline phases were found, the major one corresponding to FeAl bcc phase with a crystallite size less than 10 nm, a lattice strain up to 1.6% and a dislocation density of about 2.3 1016m-2. The other phase in low proportion was corresponding to Fe (Al,Ni) solid solution. SEM images showed an irregular morphology of powder particles.

Keywords: mechanical alloying, ternary composition, dislocation density, structural properties

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Authors: Julien Monnier, Isabelle Mouton, Francois Buy, Adrien Michel, Sylvain Ringeval, Joel Malaplate, Caroline Toffolon, Bernard Marini, Audrey Lechartier

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Chosen to design and assemble massive components for nuclear industry, the 316 Nb austenitic stainless steel (also called 316 Nb) suits well this function thanks to its mechanical, heat and corrosion handling properties. However, these properties might change during steel’s life due to thermal ageing causing changes within its microstructure. Our main purpose is to determine if the 316 Nb will keep its mechanical properties after an exposition to industrial temperatures (around 300 °C) during a long period of time (< 10 years). The 316 Nb is composed by different phases, which are austenite as main phase, niobium-carbides, and ferrite remaining from the ferrite to austenite transformation during the process. Our purpose is to understand thermal ageing effects on the material microstructure and properties and to submit a model predicting the evolution of 316 Nb properties as a function of temperature and time. To do so, based on Fe-Cr and 316 Nb phase diagrams, we studied the thermal ageing of 316 Nb steel alloys (1%v of ferrite) and welds (10%v of ferrite) for various temperatures (350, 400, and 450 °C) and ageing time (from 1 to 10.000 hours). Higher temperatures have been chosen to reduce thermal treatment time by exploiting a kinetic effect of temperature on 316 Nb ageing without modifying reaction mechanisms. Our results from early times of ageing show no effect on steel’s global properties linked to austenite stability, but an increase of ferrite hardness during thermal ageing has been observed. It has been shown that austenite’s crystalline structure (cfc) grants it a thermal stability, however, ferrite crystalline structure (bcc) favours iron-chromium demixion and formation of iron-rich and chromium-rich phases within ferrite. Observations of thermal ageing effects on ferrite’s microstructure were necessary to understand the changes caused by the thermal treatment. Analyses have been performed by using different techniques like Atomic Probe Tomography (APT) and Differential Scanning Calorimetry (DSC). A demixion of alloy’s elements leading to formation of iron-rich (α phase, bcc structure), chromium-rich (α’ phase, bcc structure), and nickel-rich (fcc structure) phases within the ferrite have been observed and associated to the increase of ferrite’s hardness. APT results grant information about phases’ volume fraction and composition, allowing to associate hardness measurements to the volume fractions of the different phases and to set up a way to calculate α’ and nickel-rich particles’ growth rate depending on temperature. The same methodology has been applied to DSC results, which allowed us to measure the enthalpy of α’ phase dissolution between 500 and 600_°C. To resume, we started from mechanical and macroscopic measurements and explained the results through microstructural study. The data obtained has been match to CALPHAD models’ prediction and used to improve these calculations and employ them to predict 316 Nb properties’ change during the industrial process.

Keywords: stainless steel characterization, atom probe tomography APT, vickers hardness, differential scanning calorimetry DSC, thermal ageing

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