Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 154

Search results for: microstructures

154 High Quality Gallium Oxide Microstructures by Catalyst-Free Thermal Oxidation

Authors: Jiang-Bei Qin, Rui-Xia Miao, Wei Ren


In this study, high crystalline gallium oxide microstructures (wires, belts, and sheets) were synthesized by catalyst-free thermal oxidation. Structural studies such as X-ray diffraction, Raman and transmission electron microscope (TEM) investigations on the microstructures showed monoclinic phase of gallium oxide and single crystalline structure. The scanning electron microscopy (SEM) observations revealed that a huge super microsheet even grows up to 450 µm in length and 206 µm in width. Gallium oxide microstructures exhibit high crystallinity along (002) and (401), respectively. The PL spectrum of these microstructures excites a blue light band centered at 441 and 489nm. The growth mechanism of gallium oxide microstructures is discussed. These gallium oxide microstructures have great potential in functional devices.

Keywords: catalyst-free, gallium oxide, microstructures, thermal oxide

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153 Microstructures of Si Surfaces Fabricated by Electrochemical Anodic Oxidation with Agarose Stamps

Authors: Hang Zhou, Limin Zhu


This paper investigates the fabrication of microstructures on Si surfaces by using electrochemical anodic oxidation with agarose stamps. The fabricating process is based on a selective anodic oxidation reaction that occurs in the contact area between a stamp and a Si substrate. The stamp which is soaked in electrolyte previously acts as a current flow channel. After forming the oxide patterns as an etching mask, a KOH aqueous is used for the wet etching of Si. A complicated microstructure array of 1 cm2 was fabricated by the method with high accuracy.

Keywords: microstructures, anodic oxidation, silicon, agarose stamps

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152 Generating 3D Battery Cathode Microstructures using Gaussian Mixture Models and Pix2Pix

Authors: Wesley Teskey, Vedran Glavas, Julian Wegener


Generating battery cathode microstructures is an important area of research, given the proliferation of the use of automotive batteries. Currently, finite element analysis (FEA) is often used for simulations of battery cathode microstructures before physical batteries can be manufactured and tested to verify the simulation results. Unfortunately, a key drawback of using FEA is that this method of simulation is very slow in terms of computational runtime. Generative AI offers the key advantage of speed when compared to FEA, and because of this, generative AI is capable of evaluating very large numbers of candidate microstructures. Given AI generated candidate microstructures, a subset of the promising microstructures can be selected for further validation using FEA. Leveraging the speed advantage of AI allows for a better final microstructural selection because high speed allows for the evaluation of many more candidate microstructures. For the approach presented, battery cathode 3D candidate microstructures are generated using Gaussian Mixture Models (GMMs) and pix2pix. This approach first uses GMMs to generate a population of spheres (representing the “active material” of the cathode). Once spheres have been sampled from the GMM, they are placed within a microstructure. Subsequently, the pix2pix sweeps over the 3D microstructure (iteratively) slice by slice and adds details to the microstructure to determine what portions of the microstructure will become electrolyte and what part of the microstructure will become binder. In this manner, each subsequent slice of the microstructure is evaluated using pix2pix, where the inputs into pix2pix are the previously processed layers of the microstructure. By feeding into pix2pix previously fully processed layers of the microstructure, pix2pix can be used to ensure candidate microstructures represent a realistic physical reality. More specifically, in order for the microstructure to represent a realistic physical reality, the locations of electrolyte and binder in each layer of the microstructure must reasonably match the locations of electrolyte and binder in previous layers to ensure geometric continuity. Using the above outlined approach, a 10x to 100x speed increase was possible when generating candidate microstructures using AI when compared to using a FEA only approach for this task. A key metric for evaluating microstructures was the battery specific power value that the microstructures would be able to produce. The best generative AI result obtained was a 12% increase in specific power for a candidate microstructure when compared to what a FEA only approach was capable of producing. This 12% increase in specific power was verified by FEA simulation.

Keywords: finite element analysis, gaussian mixture models, generative design, Pix2Pix, structural design

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151 Measurements of Physical Properties of Directionally Solidified Al-Si-Cu Ternary Alloy

Authors: Aynur Aker, Hasan Kaya


Al-12.6wt.%Si-2wt.%Cu ternary alloy of near eutectic composition was directionally solidified upward at a constant temperature gradient in a wide range of growth rates (V=8.25-165.41 µm/s). The microstructures (λ), microhardness (HV), tensile stress (σ) and electrical resistivity (ρ) were measured from directionally solidified samples. The dependence of microstructures, microhardness and electrical resistivity on growth rate (V) was also determined by statistical analysis. According to these results, it has been found that for increasing values of V, the values of HV, σ and ρ increase. Variations of electrical resistivity for casting Al-Si-Cu alloy were also measured at the temperature in range 300-500 K. The enthalpy (ΔH) and the specific heat (Cp) for the Al-Si-Cu alloy were determined by differential scanning calorimeter (DSC) from heating trace during the transformation from solid to liquid. The results obtained in this work were compared with the similar experimental results in the literature.

Keywords: Al-Si-Cu alloy, microstructures, micro-hardness, tensile stress electrical resistivity, enthalpy

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150 Comparative Studies of the Effects of Microstructures on the Corrosion Behavior of Micro-Alloyed Steels in Unbuffered 3.5 Wt% NaCl Saturated with CO2

Authors: Lawrence I. Onyeji, Girish M. Kale, M. Bijan Kermani


Corrosion problem which exists in every stage of oil and gas production has been a great challenge to the operators in the industry. The conventional carbon steel with all its inherent advantages has been adjudged susceptible to the aggressive corrosion environment of oilfield. This has aroused increased interest in the use of micro alloyed steels for oil and gas production and transportation. The corrosion behavior of three commercially supplied micro alloyed steels designated as A, B, and C have been investigated with API 5L X65 as reference samples. Electrochemical corrosion tests were conducted in an unbuffered 3.5 wt% NaCl solution saturated with CO2 at 30 0C for 24 hours. Pre-corrosion analyses revealed that samples A, B and X65 consist of ferrite-pearlite microstructures but with different grain sizes, shapes and distribution whereas sample C has bainitic microstructure with dispersed acicular ferrites. The results of the electrochemical corrosion tests showed that within the experimental conditions, the corrosion rate of the samples can be ranked as CR(A)< CR(X65)< CR(B)< CR(C). These results are attributed to difference in microstructures of the samples as depicted by ASTM grain size number in accordance with ASTM E112-12 Standard and ferrite-pearlite volume fractions determined by ImageJ Fiji grain size analysis software.

Keywords: carbon dioxide corrosion, corrosion behaviour, micro-alloyed steel, microstructures

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149 Friction Stir Processing of the AA7075T7352 Aluminum Alloy Microstructures Mechanical Properties and Texture Characteristics

Authors: Roopchand Tandon, Zaheer Khan Yusufzai, R. Manna, R. K. Mandal


Present work describes microstructures, mechanical properties, and texture characteristics of the friction stir processed AA7075T7352 aluminum alloy. Phases were analyzed with the help of x-ray diffractometre (XRD), transmission electron microscope (TEM) along with the differential scanning calorimeter (DSC). Depth-wise microstructures and dislocation characteristics from the nugget-zone of the friction stir processed specimens were studied using the bright field (BF) and weak beam dark-field (WBDF) TEM micrographs, and variation in the microstructures as well as dislocation characteristics were the noteworthy features found. XRD analysis display changes in the chemistry as well as size of the phases in the nugget and heat affected zones (Nugget and HAZ). Whereas the base metal (BM) microstructures remain un-affected. High density dislocations were noticed in the nugget regions of the processed specimen, along with the formation of dislocation contours and tangles. .The ɳ’ and ɳ phases, along with the GP-Zones were completely dissolved and trapped by the dislocations. Such an observations got corroborated to the improved mechanical as well as stress corrosion cracking (SCC) performances. Bulk texture and residual stress measurements were done by the Panalytical Empyrean MRD system with Co- kα radiation. Nugget zone (NZ) display compressive residual stress as compared to thermo-mechanically(TM) and heat affected zones (HAZ). Typical f.c.c. deformation texture components (e.g. Copper, Brass, and Goss) were seen. Such a phenomenon is attributed to the enhanced hardening as well as other mechanical performance of the alloy. Mechanical characterizations were done using the tensile test and Anton Paar Instrumented Micro Hardness tester. Enhancement in the yield strength value is reported from the 89MPa to the 170MPa; on the other hand, highest hardness value was reported in the nugget-zone of the processed specimens.

Keywords: aluminum alloy, mechanical characterization, texture characterstics, friction stir processing

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148 The Simple Two-Step Polydimethylsiloxane (PDMS) Transferring Process for High Aspect Ratio Microstructures

Authors: Shaoxi Wang, Pouya Rezai


High aspect ratio is the necessary parts of complex microstructures. Some methods available to achieve high aspect ratio requires expensive materials or complex process; others is difficult to research simple high aspect ratio structures. The paper presents a simple and cheap two-step Polydimethylsioxane (PDMS) transferring process to get high aspect ratio single pillars, which only requires covering the PDMS mold with [email protected] surface solution. The experimental results demonstrate the method efficiency and effective.

Keywords: high aspect ratio, microstructure, PDMS, Brij

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147 Predicting the Lifetime of Weathered Polyolefins by Relating Mechanics to Microstructure

Authors: Marta Chiapasco, Alexandra Porter, Finn Giuliani


Designing polymers with a specific microstructure can affect how the polymer degrades once released in the environment. Not only the amount but also the distribution of different phases determines a polymers’ degradability. The following research investigates the use of a combination of spectroscopy analysis and thermal analysis to study changes of polymers’ amorphous and crystalline phases during degradation, comparing different microstructures of polypropylene and polyethylene. The use of nanoindentation helps study how degradation proceeds across a material by looking at changes in phases, while bulk tensile test describes when the material fails. The first results demonstrate that different microstructures have different degrading rates, with homopolymer having a linear and faster degradation compared to copolymers. The goal is to create materials that degrade at faster rates without releasing microplastics into the environment.

Keywords: degradation, microstructure, nanoindentation, Raman spectroscopy

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146 Thermo-Mechanical Treatment of Chromium Alloyed Low Carbon Steel

Authors: L. Kučerová, M. Bystrianský, V. Kotěšovec


Thermo-mechanical processing with various processing parameters was applied to 0.2%C-0.6%Mn-2S%i-0.8%Cr low alloyed high strength steel. The aim of the processing was to achieve the microstructures typical for transformation induced plasticity (TRIP) steels. Thermo-mechanical processing used in this work incorporated two or three deformation steps. The deformations were in all the cases carried out during the cooling from soaking temperatures to various bainite hold temperatures. In this way, 4-10% of retained austenite were retained in the final microstructures, consisting further of ferrite, bainite, martensite and pearlite. The complex character of TRIP steel microstructure is responsible for its good strength and ductility. The strengths achieved in this work were in the range of 740 MPa – 836 MPa with ductility A5mm of 31-41%.

Keywords: pearlite, retained austenite, thermo-mechanical treatment, TRIP steel

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145 Influence of the Growth Rate on Eutectic Microstructures and Physical Properties of Aluminum–Silicon-Cobalt Alloy

Authors: Aynur Aker, Hasan Kaya


Al-12.6wt.%Si-%2wt.Co alloy was prepared in a graphite crucible under vacuum atmosphere. The samples were directionally solidified upwards with different growth rate at constant temperature gradient using by Bridgman–type growth apparatus. The values of microstructures (λ) was measured from transverse sections of the samples. The microhardness (HV), ultimate tensile strength (σ) and electrical resistivity (ρ) of the directional solidification samples were also measured. Influence of the growth rate and spacings on microhardness, ultimate tensile strength and electrical resistivity were investigated and the relationships between them were experimentally obtained by using regression analysis. The results obtained in present work were compared with the previous similar experimental results obtained for binary and ternary alloys.

Keywords: directional solidification, Al-Si-Co alloy, mechanical properties, electrical properties

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144 Microstructures Evolution of a Nano/Ultrafine Grained Low Carbon Steel Produced by Martensite Treatment Using Accumulative Roll Bonding

Authors: Mehdi Salari


This work introduces a new experimental method of martensite treatment contains accumulative roll-bonding used for producing the nano/ultrafine grained structure in low carbon steel. The ARB process up to 4 cycles was performed under unlubricated conditions, while the annealing process was carried out in the temperature range of 450–550°C for 30–100 min. The microstructures of the deformed and annealed specimens were investigated. The results showed that in the annealed specimen at 450°C for 30 or 60 min, recrystallization couldn’t be completed. Decrease in time and temperature intensified the volume fraction of the martensite cell blocks. Fully equiaxed nano/ultrafine grained ferrite was developed from the martensite cell blocks during the annealing at temperature around 500°C for 100 min.

Keywords: martensite process, accumulative roll bonding, recrystallization, nanostructure, plain carbon steel

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143 In Situ Laser-Induced Synthesis of Copper Microstructures with High Catalytic Properties and Sensory Characteristics

Authors: Maxim Panov, Evgenia Khairullina, Sergey Ermakov, Oleg Gundobin, Vladimir Kochemirovsky


The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

Keywords: laser-induced deposition, electrochemical electrodes, non-enzymatic sensors, copper

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142 Mechanical Properties and Microstructural Analysis of Al6061-Red Mud Composites

Authors: M. Gangadharappa, M. Ravi Kumar, H. N. Reddappa


The mechanical properties and morphological analysis of Al6061-Red mud particulate composites were investigated. The compositions of the composite include a matrix of Al6061 and the red mud particles of 53-75 micron size as reinforcement ranging from 0% to 12% at an interval of 2%. Stir casting technique was used to fabricate Al6061-Red mud composites. Density measurement, estimation of percentage porosity, tensile properties, fracture toughness, hardness value, impact energy, percentage elongation and percentage reduction in area. Further, the microstructures and SEM examinations were investigated to characterize the composites produced. The result shows that a uniform dispersion of the red mud particles along the grain boundaries of the Al6061 alloy. The tensile strength and hardness values increases with the addition of Red mud particles, but there is a slight decrease in the impact energy values, values of percentage elongation and percentage reduction in area as the reinforcement increases. From these results of investigation, we concluded that the red mud, an industrial waste can be used to enhance the properties of Al6061 alloy for engineering applications.

Keywords: Al6061, red mud, tensile strength, hardness and microstructures

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141 Mechanical Properties and Microstructures of the Directional Solidified Zn-Al-Cu Alloy

Authors: Mehmet Izzettin Yilmazer, Emin Cadirli


Zn-7wt.%Al-2.96wt.%Cu eutectic alloy was directionally solidified upwards with different temperature gradients (from 6.70 K/mm to 10.67 K/mm) at a constant growth rate (16.4 Km/s) and also different growth rate (from 8.3 micron/s to 166 micron/s) at a constant temperature gradient (10.67 K/mm) using a Bridgman–type growth apparatus.The values of eutectic spacing were measured from longitudinal and transverse sections of the samples. The dependency of microstructures on the G and V were determined with linear regression analysis and experimental equations were found as λl=8.953xVexp-0.49, λt=5.942xVexp-0.42 and λl=0.008xGexp-1.23, λt=0.024xGexp-0.93. The measurements of microhardness of directionally solidified samples were obtained by using a microhardness test device. The dependence of microhardness HV on temperature gradient and growth rate were analyzed. The dependency of microhardness on the G and V were also determined with linear regression analysis as HVl=110.66xVexp0.02, HVt=111.94xVexp0.02 and HVl=69.66xGexp0.17, HVt=68.86xGexp0.18. The experimental results show that the microhardness of the directionally solidified Zn-Al-Cu alloy increases with increasing the growth rate. The results obtained in this work were compared with the previous similar experimental results.

Keywords: directional solidification, eutectic alloys, microstructure, microhardness

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140 Influence of Thermal Ageing on Microstructural Features and Mechanical Properties of Reduced Activation Ferritic/Martensitic Grades

Authors: Athina Puype, Lorenzo Malerba, Nico De Wispelaere, Roumen Petrov, Jilt Sietsma


Reduced Activation Ferritic/Martensitic (FM) steels like EUROFER are of interest for first wall application in the future demonstration (DEMO) fusion reactor. Depending on the final design codes for the DEMO reactor, the first wall material will have to function in low-temperature mode or high-temperature mode, i.e. around 250-300°C of above 550°C respectively. However, the use of RAFM steels is limited up to a temperature of about 550°C. For the low-temperature application, the material suffers from irradiation embrittlement, due to a shift of ductile-to-brittle transition temperature (DBTT) towards higher temperatures upon irradiation. The high-temperature response of the material is equally insufficient for long-term use in fusion reactors, due to the instability of the matrix phase and coarsening of the precipitates at prolonged high-temperature exposure. The objective of this study is to investigate the influence of thermal ageing for 1000 hrs and 4000 hrs on microstructural features and mechanical properties of lab-cast EUROFER. Additionally, the ageing behavior of the lab-cast EUROFER is compared with the ageing behavior of standard EUROFER97-2 and T91. The microstructural features were investigated with light optical microscopy (LOM), electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM). Additionally, hardness measurements, tensile tests at elevated temperatures and Charpy V-notch impact testing of KLST-type MCVN specimens were performed to study the microstructural features and mechanical properties of four different F/M grades, i.e. T91, EUROFER97-2 and two lab-casted EUROFER grades. After ageing for 1000 hrs, the microstructures exhibit similar martensitic block sizes independent on the grain size before ageing. With respect to the initial coarser microstructures, the aged microstructures displayed a dislocation structure which is partially fragmented by polygonization. On the other hand, the initial finer microstructures tend to be more stable up to 1000hrs resulting in similar grain sizes for the four different steels. Increasing the ageing time to 4000 hrs, resulted in an increase of lath thickness and coarsening of M23C6 precipitates leading to a deterioration of tensile properties.

Keywords: ageing experiments, EUROFER, ferritic/martensitic steels, mechanical properties, microstructure, T91

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139 Study and Fine Characterization of the SS 316L Microstructures Obtained by Laser Beam Melting Process

Authors: Sebastien Relave, Christophe Desrayaud, Aurelien Vilani, Alexey Sova


Laser beam melting (LBM) is an additive manufacturing process that enables complex 3D parts to be designed. This process is now commonly employed for various applications such as chemistry or energy, requiring the use of stainless steel grades. LBM can offer comparable and sometimes superior mechanical properties to those of wrought materials. However, we observed an anisotropic microstructure which results from the process, caused by the very high thermal gradients along the building axis. This microstructure can be harmful depending on the application. For this reason, control and prediction of the microstructure are important to ensure the improvement and reproducibility of the mechanical properties. This study is focused on the 316L SS grade and aims at understanding the solidification and transformation mechanisms during process. Experiments to analyse the nucleation and growth of the microstructure obtained by the LBM process according to several conditions. These samples have been designed on different type of support bulk and lattice. Samples are produced on ProX DMP 200 LBM device. For the two conditions the analysis of microstructures, thanks to SEM and EBSD, revealed a single phase Austenite with preferential crystallite growth along the (100) plane. The microstructure was presented a hierarchical structure consisting columnar grains sizes in the range of 20-100 µm and sub grains structure of size 0.5 μm. These sub-grains were found in different shapes (columnar and cellular). This difference can be explained by a variation of the thermal gradient and cooling rate or element segregation while no sign of element segregation was found at the sub-grain boundaries. A high dislocation concentration was observed at sub-grain boundaries. These sub-grains are separated by very low misorientation walls ( < 2°) this causes a lattice of curvature inside large grain. A discussion is proposed on the occurrence of these microstructures formation, in regard of the LBM process conditions.

Keywords: selective laser melting, stainless steel, microstructure

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138 The Influence of Ni Elements on Mechanical Properties and Microstructure of Twinning Induced Plasticity (TWIP)

Authors: Yuksel Akinay, Fatih Hayat


The influence of Ni elements on mechanical properties and microstructure of twinning induced plasticity (TWIP) steels were investigated in this study. TWIP 1 (0,6C, 24Mn) and TWIP 2 (0,6C, 24Mn, 1Ni) high Mn TWIP (Twinning Induced Plasticity) steels were fabricated, and were annealed at 700°C, 800°C and 900°C for 150 minute and then air-cooled. The microstructures and mechanical properties of specimens were analysed to investigate influence of Ni element on TWIP steel. The carbide precipitations have seen in microstructure of TWIP 1 and TWIP 2 specimen annealed at 700 °C. However, the microstructures of TWIP 1 annealed at 800°C and 900°C are fully austenite and some grains are including annealing twins. However twining did not occur at TWIP 2 specimens annealed at 700 °C, 800 °C and 900 °C. TWIP 2 steel contains also Ni element differently from TWIP 1 steel. It can conclude that, Nickel (Ni) was restrained formation of twinning. The reversion of the tensile strength occurred between 700°C and 800°C because of the carbide precipitation hardening. Beside that, hardness value has decreased between 800 °C and 900 °C, which show a good agreement with the equilibrium dissolution temperature of M3C carbides. However, the results show that, carbide precipitations also are as strong barriers for the formation of twining. For this reason, twinning was not obtained at 700 °C.

Keywords: high manganese, heat treatment, SEM, TWIP steel, cold rolling, nickel

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137 Prediction of Effective Elastic and Thermal Properties of Heterogeneous Materials Using Convolutional Neural Networks

Authors: Hamdi Beji, Toufik Kanit, Tanguy Messager


The aim of this study is to develop a new method to predict the effective elastic and thermal behavior of heterogeneous materials using convolutional neural networks CNN. This work consists first of all in building a large database containing microstructures of two phases of heterogeneous material with different shapes (circular, elliptical, square, rectangular), volume fractions of the inclusion (20%, 25%, 30%), and different contrasts between the two phases in term of Young modulus and also thermal conductivity modulus (10, 100). These microstructures will be used to estimate the elastic and thermal behavior by calculating the effective bulk, shear, and thermal conductivity modulus values using a finite element method. The collected databases will be trained and tested on a deep learning model composed of a first convolutional network capable of extracting features and a second fully connected network that allows, through these parameters, to adjust the error between the found output and the expected one. The model was verified using a mean absolute percentage error (MAPE) loss function. The prediction results were excellent, with a prediction score between 92% and 98%, which justifies the good choice of the model parameters.

Keywords: numerical homogenization, convolutional neural network, deep learning, regression model

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136 Effect of Crystallographic Characteristics on Toughness of Coarse Grain Heat Affected Zone for Different Heat Inputs

Authors: Trishita Ray, Ashok Perka, Arnab Karani, M. Shome, Saurabh Kundu


Line pipe steels are used for long distance transportation of crude oil and gas under extreme environmental conditions. Welding is necessary to lay large scale pipelines. Coarse Grain Heat Affected Zone (CGHAZ) of a welded joint exhibits worst toughness because of excessive grain growth and brittle microstructures like bainite and martensite, leading to early failure. Therefore, it is necessary to investigate microstructures and properties of the CGHAZ for different welding heat inputs. In the present study, CGHAZ for two heat inputs of 10 kJ/cm and 50 kJ/cm were simulated in Gleeble 3800, and the microstructures were investigated in detail by means of Scanning Electron Microscopy (SEM) and Electron Backscattered Diffraction (EBSD). Charpy Impact Tests were also done to evaluate the impact properties. High heat input was characterized with very low toughness and massive prior austenite grains. With the crystallographic information from EBSD, the area of a single prior austenite grain was traced out for both the welding conditions. Analysis of the prior austenite grains showed the formation of high angle boundaries between the crystallographic packets. Effect of these packet boundaries on secondary cleavage crack propagation was discussed. It was observed that in the low heat input condition, formation of finer packets with a criss-cross morphology inside prior austenite grains was effective in crack arrest whereas, in the high heat input condition, formation of larger packets with higher volume of low angle boundaries failed to resist crack propagation resulting in a brittle fracture. Thus, the characteristics in a crystallographic packet and impact properties are related and should be controlled to obtain optimum properties.

Keywords: coarse grain heat affected zone, crystallographic packet, toughness, line pipe steel

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135 Production of Spherical Cementite within Bainitic Matrix Microstructures in High Carbon Powder Metallurgy Steels

Authors: O. Altuntaş, A. Güral


The hardness-microstructure relationships of spherical cementite in bainitic matrix obtained by a different heat treatment cycles carried out to high carbon powder metallurgy (P/M) steel were investigated. For this purpose, 1.5 wt.% natural graphite powder admixed in atomized iron powders and the mixed powders were compacted under 700 MPa at room temperature and then sintered at 1150 °C under a protective argon gas atmosphere. The densities of the green and sintered samples were measured via the Archimedes method. A density of 7.4 g/cm3 was obtained after sintering and a density of 94% was achieved. The sintered specimens having primary cementite plus lamellar pearlitic structures were fully quenched from 950 °C temperature and then over-tempered at 705 °C temperature for 60 minutes to produce spherical-fine cementite particles in the ferritic matrix. After by this treatment, these samples annealed at 735 °C temperature for 3 minutes were austempered at 300 °C salt bath for a period of 1 to 5 hours. As a result of this process, it could be able to produced spherical cementite particle in the bainitic matrix. This microstructure was designed to improve wear and toughness of P/M steels. The microstructures were characterized and analyzed by SEM and micro and macro hardness.

Keywords: powder metallurgy steel, bainite, cementite, austempering and spheroidization heat treatment

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134 Finite Element Analysis of Mechanical Properties of Additively Manufactured 17-4 PH Stainless Steel

Authors: Bijit Kalita, R. Jayaganthan


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

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

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133 Selective Laser Melting (SLM) Process and Its Influence on the Machinability of TA6V Alloy

Authors: Rafał Kamiński, Joel Rech, Philippe Bertrand, Christophe Desrayaud


Titanium alloys are among the most important material in the aircraft industry, due to its low density, high strength, and corrosion resistance. However, these alloys are considered as difficult to machine because they have poor thermal properties and high reactivity with cutting tools. The Selective Laser Melting (SLM) process becomes even more popular through industry since it enables the design of new complex components, that cannot be manufactured by standard processes. However, the high temperature reached during the melting phase as well as the several rapid heating and cooling phases, due to the movement of the laser, induce complex microstructures. These microstructures differ from conventional equiaxed ones obtained by casting+forging. Parts obtained by SLM have to be machined in order calibrate the dimensions and the surface roughness of functional surfaces. The ball milling technique is widely applied to finish complex shapes. However, the machinability of titanium is strongly influenced by the microstructure. So the objective of this work is to investigate the influence of the SLM process, i.e. microstructure, on the machinability of titanium, compared to conventional forming processes. The machinability is analyzed by measuring surface roughness, cutting forces, cutting tool wear for a range of cutting conditions (depth of cut ap, feed per tooth fz, spindle speed N) in accordance with industrial practices.

Keywords: ball milling, microstructure, surface roughness, titanium

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132 Critical Study on the Sensitivity of Corrosion Fatigue Crack Growth Rate to Cyclic Waveform and Microstructure in Marine Steel

Authors: V. C. Igwemezie, A. N. Mehmanparast


The primary focus of this work is to understand how variations in the microstructure and cyclic waveform affect the corrosion fatigue crack growth (CFCG) in steel, especially in the Paris region of the da/dN vs. ΔK curve. This work is important because it provides fundamental information on the modelling, design, selection, and use of steels for various engineering applications in the marine environment. The corrosion fatigue tests data on normalized and thermomechanical control process (TMCP) ferritic-pearlitic steels by the authors were compared with several studies on different microstructures in the literature. The microstructures of these steels are radically different and general comparative fatigue crack growth resistance performance study on the effect of microstructure in these materials are very scarce and where available are limited to few studies. The results, for purposes of engineering application, in this study show less dependency of fatigue crack growth rate (FCGR) on yield strength, tensile strength, ductility, frequency and stress ratio in the range 0.1 – 0.7. The nature of the steel microstructure appears to be a major factor in determining the rate at which fatigue cracks propagate in the entire da/dN vs. ΔK sigmoidal curve. The study also shows that the sine wave shape is the most damaging fatigue waveform for ferritic-pearlitic steels. This tends to suggest that the test under sine waveform would be a conservative approach, regardless of the waveform for design of engineering structures.

Keywords: BS7910, corrosion-fatigue crack growth rate, cyclic waveform, microstructure, steel

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131 Rheological Study of Chitosan/Montmorillonite Nanocomposites: The Effect of Chemical Crosslinking

Authors: K. Khouzami, J. Brassinne, C. Branca, E. Van Ruymbeke, B. Nysten, G. D’Angelo


The development of hybrid organic-inorganic nanocomposites has recently attracted great interest. Typically, polymer silicates represent an emerging class of polymeric nanocomposites that offer superior material properties compared to each compound alone. Among these materials, complexes based on silicate clay and polysaccharides are one of the most promising nanocomposites. The strong electrostatic interaction between chitosan and montmorillonite can induce what is called physical hydrogel, where the coordination bonds or physical crosslinks may associate and dissociate reversibly and in a short time. These mechanisms could be the main origin of the uniqueness of their rheological behavior. However, owing to their structure intrinsically heterogeneous and/or the lack of dissipated energy, they are usually brittle, possess a poor toughness and may not have sufficient mechanical strength. Consequently, the properties of these nanocomposites cannot respond to some requirements of many applications in several fields. To address the issue of weak mechanical properties, covalent chemical crosslink bonds can be introduced to the physical hydrogel. In this way, quite homogeneous dually crosslinked microstructures with high dissipated energy and enhanced mechanical strength can be engineered. In this work, we have prepared a series of chitosan-montmorillonite nanocomposites chemically crosslinked by addition of poly (ethylene glycol) diglycidyl ether. This study aims to provide a better understanding of the mechanical behavior of dually crosslinked chitosan-based nanocomposites by relating it to their microstructures. In these systems, the variety of microstructures is obtained by modifying the number of cross-links. Subsequently, a superior uniqueness of the rheological properties of chemically crosslinked chitosan-montmorillonite nanocomposites is achieved, especially at the highest percentage of clay. Their rheological behaviors depend on the clay/chitosan ratio and the crosslinking. All specimens exhibit a viscous rheological behavior over the frequency range investigated. The flow curves of the nanocomposites show a Newtonian plateau at very low shear rates accompanied by a quite complicated nonlinear decrease with increasing the shear rate. Crosslinking induces a shear thinning behavior revealing the formation of network-like structures. Fitting shear viscosity curves via Ostward-De Waele equation disclosed that crosslinking and clay addition strongly affect the pseudoplasticity of the nanocomposites for shear rates γ ̇>20.

Keywords: chitosan, crossliking, nanocomposites, rheological properties

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130 Microstructures and Chemical Compositions of Quarry Dust As Alternative Building Material in Malaysia

Authors: Abdul Murad Zainal Abidin, Tuan Suhaimi Salleh, Siti Nor Azila Khalid, Noryati Mustapa


Quarry dust is a quarry end product from rock crushing processes, which is a concentrated material used as an alternative to fine aggregates for concreting purposes. In quarrying activities, the rocks are crushed into aggregates of varying sizes, from 75mm until less than 4.5 mm, the size of which is categorized as quarry dust. The quarry dust is usually considered as waste and not utilized as a recycled aggregate product. The dumping of the quarry dust at the quarry plant poses the risk of environmental pollution and health hazard. Therefore, the research is an attempt to identify the potential of quarry dust as an alternative building material that would reduce the materials and construction costs, as well as contribute effort in mitigating depletion of natural resources. The objectives are to conduct material characterization and evaluate the properties of fresh and hardened engineering brick with quarry dust mix proportion. The microstructures of quarry dust and the bricks were investigated using scanning electron microscopy (SEM), and the results suggest that the shape and surface texture of quarry dust is a combination of hard and angular formation. The chemical composition of the quarry dust was also evaluated using X-ray fluorescence (XRF) and compared against sand and concrete. The quarry dust was found to have a higher presence of alumina (Al₂O₃), indicating the possibility of an early strength effect for brick. They are utilizing quarry dust waste as replacement material has the potential of conserving non-renewable resources as well as providing a viable alternative to disposal of current quarry waste.

Keywords: building materials, cement replacement, quarry microstructure, quarry product, sustainable materials

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129 Fabrication of Hybrid Scaffolds Consisting of Cell-laden Electrospun Micro/Nanofibers and PCL Micro-structures for Tissue Regeneration

Authors: MyungGu Yeo, JongHan Ha, Gi-Hoon Yang, JaeYoon Lee, SeungHyun Ahn, Hyeongjin Lee, HoJun Jeon, YongBok Kim, Minseong Kim, GeunHyung Kim


Tissue engineering is a rapidly growing interdisciplinary research area that may provide options for treating damaged tissues and organs. As a promising technique for regenerating various tissues, this technology requires biomedical scaffolds, which serve as an artificial extracellular matrix (ECM) to support neotissue growth. Electrospun micro/nanofibers have been used widely in tissue engineering because of their high surface-area-to-volume ratio and structural similarity to extracellular matrix. However, low mechanical sustainability, low 3D shape-ability, and low cell infiltration have been major limitations to their use. In this work, we propose new hybrid scaffolds interlayered with cell-laden electrospun micro/nano fibers and poly(caprolactone) microstructures. Also, we applied various concentrations of alginate and electric field strengths to determine optimal conditions for the cell-electrospinning process. The combination of cell-laden bioink (2 ⅹ 10^5 osteoblast-like MG63 cells/mL, 2 wt% alginate, 2 wt% poly(ethylene oxide), and 0.7 wt% lecithin) and a 0.16 kV/mm electric field showed the highest cell viability and fiber formation in this process. Using these conditions and PCL microstructures, we achieved mechanically stable hybrid scaffolds. In addition, the cells embedded in the fibrous structure were viable and proliferated. We suggest that the cell-embedded hybrid scaffolds fabricated using the cell-electrospinning process may be useful for various soft- and hard-tissue regeneration applications.

Keywords: bioink, cell-laden scaffold, micro/nanofibers, poly(caprolactone)

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128 Analysis of Thermal Effect on Functionally Graded Micro-Beam via Mixed Finite Element Method

Authors: Cagri Mollamahmutoglu, Ali Mercan, Aykut Levent


Studies concerning the microstructures are becoming more important as the utilization of various micro-electro mechanical systems (MEMS) are increasing. Thus in recent years, thermal buckling and vibration analysis of microstructures have been subject to many investigations that are utilizing different numerical methods. In this study, thermal effects on mechanical response of a functionally graded (FG) Timoshenko micro-beam are presented in the framework of a mixed finite element formulation. Size effects are taken into consideration via modified couple stress theory. The mixed formulation is based on a function which in turn is derived via Gateaux Differential scientifically. After the resolution of all field equations of the beam, a potential operator is carefully constructed. Then this operator is used for the manufacturing of the functional. Usual procedures of finite element approximation are utilized for the derivation of the mixed finite element equations once the potential is obtained. Resulting finite element formulation allows usage of C₀ type simple linear shape functions and avoids shear-locking phenomena, which is a common shortcoming of the displacement-based formulations of moderately thick beams. The developed numerical scheme is used to obtain the effects of thermal loads on the static bending, free vibration and buckling of FG Timoshenko micro-beams for different power-law parameters, aspect ratios and boundary conditions. The versatility of the mixed formulation is presented over other numerical methods such as generalized differential quadrature method (GDQM). Another attractive property of the formulation is that it allows direct calculation of the contribution of micro effects on the overall mechanical response.

Keywords: micro-beam, functionally graded materials, thermal effect, mixed finite element method

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127 Effect of Microstructure on Transition Temperature of Austempered Ductile Iron (ADI)

Authors: A. Ozel


The ductile to brittle transition temperature is a very important criterion that is used for selection of materials in some applications, especially in low-temperature conditions. For that reason, in this study transition temperature of as-cast and austempered unalloyed ductile iron in the temperature interval from -60 to +100 degrees C have been investigated. The microstructures of samples were examined by light microscope. The impact energy values obtained from the experiments were found to depend on the austempering time and temperature.

Keywords: Austempered Ductile Iron (ADI), Charpy test, microstructure, transition temperature

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126 Short and Long Crack Growth Behavior in Ferrite Bainite Dual Phase Steels

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


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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125 Metallograpy of Remelted A356 Aluminium following Squeeze Casting

Authors: Azad Hussain, Andrew Cobley


The demand for lightweight parts with high mechanical strength(s) and integrity, in sectors such as the aerospace and automotive is ever increasing, motivated by the need for weight reduction in order to increase fuel efficiency with components usually manufactured using a high grade primary metal or alloy. For components manufactured using the squeeze casting process, this alloy is usually A356 aluminium (Al), it is one of the most versatile Al alloys; and is used extensively in castings for demanding environments. The A356 castings provide good strength to weight ratio making it an attractive option for components where strength has to be maintained, with the added advantage of weight reduction. In addition, the versatility in castabilitiy, weldability and corrosion resistance are other attributes that provide for the A356 cast alloy to be used in a large array of industrial applications. Conversely, it is rare to use remelted Al in these cases, due the nature of the applications of components in demanding environments, were material properties must be defined to meet certain specifications for example a known strength or ductility. However the use of remelted Al, especially primary grade Al such as A356, would offer significant cost and energy savings for manufacturers using primary alloys, provided that remelted aluminium can offer similar benefits in terms of material microstructure and mechanical properties. This study presents the results of the material microstructure and properties of 100% primary A356 Al and 100% remelt Al cast, manufactured via the direct squeeze cast method. The microstructures of the castings made from remelted A356 Al were then compared with the microstructures of primary A356 Al. The outcome of using remelting Al on the microstructure was examined via different analytical techniques, optical microscopy of polished and etched surfaces, and scanning electron microscopy. Microstructural analysis of the 100% remelted Al when compared with primary Al show similar α-Al phase, primary Al dendrites, particles and eutectic constituents. Mechanical testing of cast samples will elucidate further information as to the suitability of utilising 100% remelt for casting.

Keywords: A356, microstructure, remelt, squeeze casting

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