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This volume comprises the select proceedings of FiMPART 2015. The volume covers advances in major areas of materials research under one umbrella. This volume covers all aspects of materials research, processing, fabrication, structure/property evaluation, applications of ferrous, non-ferrous, ceramic, polymeric materials and composites including biomaterials, materials for energy, fuel cells/hydrogen storage technologies, batteries, super-capacitors, nano-materials for energy and structural applications, aerospace structural metallic materials, bulk metallic glasses and other advanced materials. The book will be useful to researchers, students, and professional working in areas related to materials innovation and applications.



Chapter 1. String-Like Fiber Dust Occurrence in Crush Cutting of Stacked Liner Boards

To convert a corrugated fiberboard (Cfb) into a couple of unfolded formed-cut sheets for making a container box, since the raw Cfb is cut off by using a combination of center-bevelled (wedge) blade and its counter faceplate, the cutting edge of blade dynamically and repeatedly collides on the faceplate. Therefore, the edge profile of blade and the contact zone of faceplate plastically deform and abrasively removed with respect to the repeated cutting times. When the cutting times of raw Cfb increase and reach a certain number, the occurrence probability of string-like dust empirically increases due to the variation of edge profile of blade and dent of faceplate. When such the string-like dusts become larger and adhere to the product object, they become foreign matter. Therefore, in order to reduce the occurrence of string-like dusts, any countermeasures are required. Nagasawa et al. (J Jpn Soc Technol Plast (SOSEI-TO-KAKOU) 43(498):624–628, 2002, [3]) had reported about the effects of blade tip thickness on string-like dust occurrence in the case of white-coated paperboard of basis weight 350 (a thickness of 0.45 mm) and the correlation between room humidity and dust occurrence probability. However, any generation mechanism of string-like dusts and its applicability of occurrence estimation to a Cfb are not sufficiently discussed in the past. When the Cfb is subjected to a pressure cutting of flatbed die cutter, a stacked collection of three raw fiber sheets, upper liner, medium, and lower liner sheets, is fasten and cut off by a wedge indentation. These raw sheets have a thickness of 0.18–0.22 mm, which is relatively thinner than that of widely known white-coated paper of 0.45 mm, and these three raw sheets have different mechanical properties for each layer. Synthetically, the occurrence probability of string-like dusts in the Cfb cutting appears to be partially different from that of the white-coated paperboard. The authors experimentally investigated the relationship between the blade tip thickness and geometrical features of string-like dusts and the corresponded cutting load responses, in order to reveal the mechanical condition for causing the string-like dusts.

Shigeru Nagasawa, Takuya Oyake, Takashi Kajizuka

Chapter 2. Phase Transformation of Amorphous Rice Husk Silica

This work aims at assessing the crystallization process of amorphous silica from rice husk (RH) by in situ X-ray diffraction, upon heating up to 1450 °C in a high-temperature chamber. The study includes microstructural characterization by transmission electron microscopy. The work was conducted on rice husk ash (RHA), obtained by combustion of RH at 650 °C with and without leaching in 1 N HCl solution, obtaining samples with variable impurity content. The results showed that crystallization of RHA amorphous silica upon continuous heating occurred at higher temperatures compared to the isothermal one, considering the sample purity. The type of polymorph silica identified in the samples during continuous heating consisted of cristobalite or a combination of cristobalite and tridymite depending on the impurity levels in the samples. The study revealed silica crystallites with spherical shape nucleated by a dominant homogeneous mechanism. The size of crystallites ranges from around 2 nm to 20 nm. Larger particles nucleated on impurities and constituted by combinations of P, Ca, K, Mg, and Na were also observed.

A. L. Rivas, Grace Vera, Víctor Palacios, Mauricio Cornejo, Andrés Rigail, Guillermo Solórzano

Chapter 3. Analysis of Nano/Micro Bimodal SUS316L Powder Behavior

The components fabricated with nanopowder tend to show better surface roughness and mechanical properties with low sintering temperature. However, at the same time, its high price and reactivity are critical problems of nanopowder. Thus, nano/micro bimodal powder has been introduced in powder process to minimize the problems of nanopowder. In this research, the effect of nanopowder content in nano/micro bimodal powder has been investigated. Bimodal powder was prepared with 100-nm and 4-μm-sized stainless steel 316L powder. They were mixed into 5 grades depend on nanopowder volume ratio from 0 to 100%. The apparent and tap density of the powders were measured, and their flowability was compared with Hausner ratio. Unlike theoretical calculation, the tap density of bimodal powders did not show the packing effect due to distribution of nanoparticles. The compaction behavior was also investigated to verify the bimodal packing effect. The result indicated that the bimodal powder with 25 vol. % nanopowder had the highest relative density.

Joo Won Oh, Ravi Bollina, Won Sik Lee, Seong Jin Park

Chapter 4. Tensile Deformation Behavior of Al-rich Ferritic Steels for Advanced Light Water Reactors

Following the Fukushima Daiichi incident, there has been considerable interest in developing accident-tolerant fuel cladding materials to make light water reactors (LWRs) more resistant to such accidents. Traditionally, zirconium-based alloys are used as the fuel cladding material in these reactors. Exothermic reaction with steam under accident conditions may lead to production of hydrogen with the possibility of catastrophic consequences. Hence, aluminum-rich (around 5 wt%) ferritic steels such as FeCralloy, APMTTM and APMTM have potential for accident-tolerant fuel cladding applications. These materials create an aluminum-based oxide scale protecting the alloy at elevated temperatures. Tensile deformation behavior of FeCralloy and APMTTM alloy was compared at different temperatures (25–500 °C) and strain rates, and correlated with microstructural characteristics. Serrations appeared in the stress–strain curves of these alloys tested in a limited temperature range (300–400 °C). Presence of serrations did not lead to a decrease in elongation to fracture despite showing negative strain rate sensitivity behavior. The appearance of serrations is explained on the basis of dynamic strain aging (DSA) effect due to solute–dislocation interactions.

Ankan Guria, Indrajit Charit, Bojan Petrovic

Chapter 5. A Study on Precipitation Behavior of A356 Alloy by Ultrasonic Velocity Measurements

Al-356 alloy is an aluminum alloy of Al-7Si-0.3 Mg. The effect of solutionizing condition and precipitation hardening on microstructure of this alloy is investigated. The microstructure of a given alloy has a bearing on its mechanical properties. Thus, in the present case, a study on the effect of above parameters, namely solutionizing and precipitation hardening on microstructure (optical, SEM), and hardness and ultrasonic velocity (longitudinal velocity), has been made. In the age-hardening process, the precipitates appear in the form of clusters. Nature of distribution of these clusters contributes significantly toward variation in the bulk material of the alloy. In the present investigation, the behavior of solutionizing and aging treatment under varying conditions of temperature and time that result in the morphological changes in microstructure, and ultrasonic velocity for the A356 alloy have been reported.

G. V. S. Murthy

Chapter 6. Synthesis of Superhard Lightweight Composites and Improvement of Their Properties via Chemical Processing

Superhard lightweight composites were prepared by self-propagating high-temperature synthesis (SHS), attrition milling, chemical leaching in concentrated HCl and/or HNO3 acids and spark plasma sintering (SPS) under N gas pressure. Such processing features were conducted for production of the superhard B13C2, B11.72C3.28, c-BN and c-BC2N chemical compounds in the B4C(67 wt%)-Al/WC-Co/Cu-based composite. The materials were studied by X-ray diffraction, scanning electron microscope equipped with energy-dispersive spectrometer system (SEM-EDS) and also with microindentation and nanoindentation of composites. During SHS, the B4C was partly transformed into boron-rich B13C2 boron carbide in quantity of ~60 wt%. The c-BC2N content in the composite was ~12 wt% after heat treatment of SHS-composite under nitrogen gas flow at temperature of 850 °C for 2 h. Subsequently, the disintegrated and attrition-milled powdered SHS-composite was chemically leached, and as result, the soft Al-containing compounds were reduced from ~27 wt% to ~4 wt%. During SPS, the boron-rich B13C2 boron carbide was transformed into carbon-rich B11.72C3.28 boron carbide in quantity of ~87 wt%. The maximal Vickers microhardness of superhard composites was ~4400 HV1.0 (~46 GPa). The composite has high thermal stability and chemical inertness.

Lembit Kommel, Toomas Tamm, Raido Metsvahi, Kadri Nokkur

Chapter 7. Structural and Chemical Variations Induced by Thermomechanical Cycling in Shape Memory Ac-tuators

Lamellar thermal actuators, for temperature control in hydraulic systems, were manufactured from a Cu-Zn-Al shape memory alloy (SMA) and trained in bending, between 100 and 500 cycles. Training comprised electrical heating in still air and ventilated air-cooling during which a load, fastened at actuator’s free end, was lifted by shape memory effect (SME) and lowered due to the softening caused by martensite formation, respectively. The structural effects of training, evaluated by differential scanning calorimetry (DSC), optical (OM), scanning electron (SEM), and atomic force microscopy (AFM), consisted in a raising tendency of critical transformation temperatures of martensite reversion to parent phase and in a noticeable decrease of surface micro-relief, since the average widths and heights of martensite plates decreased almost seven and four times, respectively. Trained actuators, able to develop two-way shape memory effect (TWSME) by reducing their curvature (partial straightening) during heating and by recovering it (partial curving) during cooling, were thermally cycled in oil, in a hydraulic installation. Temperature variations versus time, recorded during thermal cycling performed in oil, revealed the influences of: (i) the number of training cycles; (ii) overheating caused by oil thermal inertia, and (iii) heating interruption during martensite reversion to parent phase. Heating interruption, associated with temperature memory effect, caused the occurrence of two martensite populations, during subsequent cooling, as substantiated by OM, SEM, and AFM observations. Due to repetitive displacement of parent phase/austenite interface, during heating-cooling performed on training and subsequent oil-cycling, fluctuations of chemical composition were detected by energy dispersive X-ray spectroscopy (EDS) mapping, under the form of differences between maximum and minimum local chemical compositions.

Leandru-Gheorghe Bujoreanu, Bogdan Pricop, Nicoleta Monica Lohan, Marius-Gabriel Suru, Bogdan Istrate

Chapter 8. Thermal Conductivity on Ternary Eutectic Fatty Acid as Phase Change Material (PCM) by Various Treated Exfoliated Graphite Nanoplatelets (xGnP)

Today’s power infrastructure involves unpredictability in both supply and demand, that is, difficult to manage. Energy storage is an essential method to keep the sustainable energy in stable condition. This work is focused on developing ternary eutectic fatty acid like capric-myristic-palmitic acid (CA-MA-PA) mixture as PCM and increases their property by two different kinds of exfoliated graphite nanoplatelets (xGnP-s and xGnP-m) were mixed uniformly under the assistance of ultrasonication in the mass fractions of 5 and 10% for latent heat thermal energy storage. Initially, graphite was surface modified by concentration of solar energy with a Fresnel lens in open atmosphere, then exfoliation of graphite nanoplatelets by solar irradiation (xGnP-s), and exfoliation of graphite nanoplatelets by Microwave irradiation (xGnP-m) in a short time on the ratio of 10:1 (10 for surface modification then 1 for exfoliation). The investigation of structure, thermal energy storage properties, and thermal conductivity of novel composite PCM with these two nanoplatelets was performed. The structural evolution was probed using scanning electron microscope (SEM). The thermal conductivity of the samples in liquid phase was measured using the transient line source method like KD2Pro. The energy storage properties, including melting/solidification temperatures and enthalpies, were measured using a differential scanning calorimeter. It was shown that the presence of the xGnP decreases the phase change enthalpies and temperatures. Furthermore, CA-MA-PA+10% xGnP-s has slightly change then ternary eutectic CA-MA-PA PCM in phase change enthalpies and temperature (Tm = 17.1 °C; ΔHm = 142.2 J/g) for melting, (Tf = 9.7 °C; ΔHf = 139.5 J/g) for freezing respectively, while CA-MA-PA+10% xGnP-m showed higher thermal conductivity 0.209 W/mK which increased up to 140%.

B. Eanest Jebasingh

Chapter 9. Elements Diffusion in Brazing Seam of High Volume Fraction SiCp/6063Al Matrix Composites

In this research, 6063 aluminum matrix composites containing 55–75% SiC particle reinforcing phase was selected as the parent metal and Al-Cu24-Si5-Zn2-Ti1 alloy metal was selected as the filler metal. After nickel plating of the parent metal, the brazing process is carried out on vacuum brazing furnace under the temperature of 565, 570, and 575 °C and holding for 10, 20, and 30 min. The interfacial microstructure is investigated by light optical microscopy (LOM) and scanning electron microscopy (SEM), and the element diffusion is analyzed by energy spectrum analysis (EDS). The result shows that the nickel plating layer on the surface of parent metal not only metalizes the SiC particle, but also participates in the diffusion process. The element distribution in the brazing seam is described exactly. Finally, the reason why finest crystalline grains and evenest distribution could be achieved under brazing temperature of 575 °C and holding for 30 min is analyzed.

Dongfeng Cheng, Jitai Niu, Zeng Gao, Josip Brnic

Chapter 10. Functionally Graded Cemented Carbides Elaboration by Imbibition Process—Better Understanding of Liquid Migration and Homogenization Mechanisms for an Improved Process

Cemented carbides are used in rock drilling, for mining tools and other wear-resistant parts. These composite materials possess an excellent compromise between hardness and toughness. Currently, the concept of graded structure (FGM) is widely studied to improve these two properties simultaneously, and thus to increase the service life of drilling tools. This paper focuses on the imbibition process. The imbibition process gradually enriches the core of dense cemented carbide with binder phase and is based on the principle of liquid-phase migration in a solid/liquid body. FGM generated by such techniques shows interesting mechanical properties gradient, such as 400 HV on 20 mm hardness gradient. Hardness gradient development is achieved through a better understanding of kinetics and other phenomena occurring during imbibition. The goal is to select suitable process parameter for each grade of carbide.

O. Ther, C. Colin, A. Dourfaye

Chapter 11. Water Analogy Experiment on the Multi-concentration Pouring Process of a 585 Ton Steel Ingot

Multi-concentration pouring is applied to reduce the macrosegregation in heavy ingots in production, in which ladles with different carbon contents are used to realize initial inverse macrosegregation after pouring so as to offset the macrosegregation occurring during solidification. However, it’s not yet clear how carbon redistributes in the melt during pouring. A water analogy experiment platform was constructed to investigate the carbon transportation during pouring for heavy steel ingots. The pouring of a 585t steel ingot by five ladles of different carbon contents was investigated by water analogy method. Methyl blue was adopted as solute. Array of 24 probes were used to measure the solute concentration at different locations in the ingot mold. The results show that an initial inverse macrosegregation of carbon is achieved at the end of pouring, positive segregation at the bottom and negative at the top. But, mixing happens in both tundish and ingot mold during filling, therefore, the bottom positive segregation is only a half of the designed one based on the carbon content difference of the ladles.

Jinwu Kang, Chi Zhang, Chao Dong, Houfa Shen, Baicheng Liu

Chapter 12. Ferroelectric (Hf, Zr)O2 Thin Films for High-Density Nonvolatile Memories

In the field of ferroelectric nonvolatile memories, the density enhancement approached the limit due to the scaling issues of perovskite-based ferroelectrics and complicated processing steps involved. However, the unexpected discovery of ferroelectricity in solid solutions of hafnium and zirconium binary oxides renewed the interest in high-density ferroelectric-based nonvolatile memories. This is mainly due to the familiarity of HfO2 and ZrO2 as a high-k dielectric material in advanced semiconductor devices and its CMOS compatibility. In this context, hafnium zirconate (HfZrO2) thin films were prepared on Pt/Al2O3/SiO2/Si substrates by radio frequency (rf) magnetron sputtering using a stoichiometric (Hf, Zr)O2 ceramic target. Fine-grained surface morphology for 500 °C deposited HfZrO2 films and rms roughness comparable to the underlying Pt surface were observed with atomic force microscopy (AFM). Films deposited at 500–750 °C showed typical hysteresis loop (phase angle vs. applied voltage) in the piezo force microscopy (PFM) studies, confirming the ferroelectric property of the film. Also, the stabilization of the ferroelectric phase at 500 °C is advantageous for the CMOS compatibility with TiN bottom/top electrodes .

F. Ambriz-Vargas, R. Thomas, A. Ruediger

Chapter 13. Advanced System for Nanofabrication and Nanomanipulation Based on Shape Memory Alloy

Miniaturization is the central theme in modern fabrication technology. Many of the components used in modern products are becoming smaller and smaller. Here it is reported about the frontier nano-assembling and nano-investigations using new practical 3-D nanomanipulation system based on advanced high precision piezoelectric resonance motors, and the bimetallic composite nanotweezers based on Ti2NiCu alloy with shape memory effect. The system for the first time gives the real possibility for high-speed three-dimensional controllable reproducible, manipulation and fabrication of large-scale nanostructures in SEM, TEM, SEM, FIM microscopes under vacuum, air and liquid conditions. The system can manipulate real nano-objects, i.e., nanotubes and bio-nanoparticles. The size of the objects to be manipulated: 30–1000 nm; the motion range—15 mm, the minimal step—0.4 to 10 nm, the thermal drift <5 nm/h at 20 °C; the speed of linear motion: 20–20 mm/s. The experimental design and test of the new generation nanotools based on original bilayer Ti2NiCu/Pt composite structures is described. The production technology is based on standard ion beam nanofabrication technology for full cycle of operational stages of practical nanotweezers production with record small dimensions: (3–20) × (2–3) × 1.6 μm3. The technological experiments were done by usage of a novel focused ion beam instrument Raith ionLiNETM. ionLiNETM Raith was applied for experimental composite nanotweezers production on the base of Ti2NiCu/W with length—30 μm, gap width 0.9 μm. The tests showed high quality of reproduction and long-term operation of nanotweezers under thermal control at temperature change only 14 K.

S. von Gratowski, V. Koledov, V. Shavrov, S. Petrenko, A. Irzhak, A. Shelyakov, R. Jede

Chapter 14. Synthesis of Aluminium–Graphene Nanocomposite Sintered Using Spark Plasma Sintering

Graphene (Gr) has attracted tremendous attention for the synthesis of lightweight structural nanocomposites due to its excellent properties such as high Young’s modulus (1 TPa), high fracture strength (~125 GPa) and extreme thermal conductivity (~5000 W/m/K). Fabrication of pure aluminium–graphene nanocomposite is conducted using a chemical synthesis route followed by consolidation using spark plasma sintering process. The pure aluminium powder was initially cryomilled to refine the grain structure. Subsequently, nanocomposites of Al-reduced graphene (Al-Gr) were synthesized using a chemical method employing different proportions (by volume fraction) of graphene oxide (GO) dispersed in pure aluminium powder. The synthesized powder was ball milled under optimized conditions followed by spark plasma sintering. The powder and sintered Al-Gr nanocomposites are characterized by X-ray diffraction, Raman spectroscopy, SEM and TEM microscopy. The mechanical behaviour is evaluated using the indentation hardness method. GO was found fully converted to reduced graphene during SPS. The increased proportion of reduced graphene in aluminium powder has suggested improved mechanical properties such as hardness after SPS. The structure–property correlation of synthesized Al-Gr nanocomposites is discussed with regard to the improvement in the mechanical behaviour.

Vipin Jain, Anil Kumar, Bathula Sivaiah, Ajay Dhar

Chapter 15. Time-Lapse Correlative 3D Imaging Applied to the Corrosion Study of AZ31 Mg Alloy in a Saline Environment

In the present study, time-evolved (4D) correlative 3D imaging techniques, combining microtomography and nanotomography with 3D FIB-SEM sectioning and EDS, have allowed shedding light on morphological and compositional aspects of the corrosion behaviour of AZ31 magnesium alloy. By applying these techniques, the corrosion processes involved, corrosion stages I, II and III, were identified successfully despite the challenging fast corrosion behaviour of magnesium-based alloys. The 3D reconstruction confirmed the near-surface restriction of the filiform corrosion (stage II) and the subsequent severe inward corrosion during stage III. Furthermore, the distribution of the coarse Al–Mn intermetallic particles could be correlated with the corrosion front development.

H. M. Krebs, Ali Chirazi, L. Lechner, J. Gelb, X. Zhou, G. E. Thompson, P. J. Withers

Chapter 16. Welding and Heat Treatment Behaviour of T23 (2.25Cr-1.6W-V-Nb) Steel Tubes in Power Plant Applications

T23 (2.25Cr-1.6W-V-Nb) is a creep strength enhanced ferritic (CSEF) steel tube for high-temperature thermal power plant applications. Initially, the material was expected to be similar or superior to SA 213 T22 in weldability aspects, but with enhanced creep properties. The lower-carbon, bainitic steel weldment with expected peak hardness below 350 HV in the as-welded condition meant the elimination of any preheat or post-weld heat treatments. The material was also not expected to be prone to cold cracks, hot cracks, stress relief cracks, stress corrosion cracks and brittle fractures. But, subsequent practical experience has suggested otherwise; and there is a need to amend the original presumptions, especially when used in high-restraint panel-welded power plant applications. This paper revisits these and makes a consolidation of the technological discipline needed in the fabrication of this material. The influence of preheat and PWHT on the microstructure and hardness of the SMAW and GTAW welded T23 steel are investigated. Implant weldability test and environment-assisted cracking test helped understand delayed cracking issues and find the optimum preheat temperature. Using Gleeble thermo-mechanical simulation, CCT diagrams were constructed for HAZ. Stress relief cracking susceptibility test was done using physical simulator to find out optimum PWHT temperature. The effect of various cooling rates after normalising treatment of cold bent tubes on toughness has also been studied through Gleeble. The paper thus draws a guideline for the fabrication of components, especially under high restraint such as panel-welded applications.

R. Easwaran, G. Vimalan, R. Ravibharath, P. Sundaramoorthy, N. Raju, G. Ravichandran

Chapter 17. Solar Performance Analysis of ZrOx/ZrC-ZrN/Zr/SS Spectrally Selective Coating Under Extreme Thermal Environment

ZrOx/ZrC-ZrN/Zr absorber-reflector tandem solar selective coatings (ARTSSCs) on stainless steel (SS) substrates are investigated under extreme thermal conditions. The deposited coatings are heated upto 900 °C at 5 °C/min heating rate in nitrogen and air environments to explore the structure-property correlation and their impact on thermal degradation. We observed that tetragonal, monoclinic and cubic zirconium oxide phases are present only for heat-treated ARTSSC structures, suggesting the partial conversion of nitride and carbide phases from absorbers layer of as-deposited structures. Surface roughness ~13.75 nm, in as-deposited structures, has increased upto 22.67 ± 0.05 nm and 26.21 ± 0.08 nm in nitrogen and air heat-treated coatings, respectively. This increased surface roughness and dominant zirconium oxide phases, in heat-treated ARTSSCs, resulted into poor hardness ~13.3 GPa and ~6.64 GPa for samples heat treated in nitrogen and air ambient, with respect to ~18.88 GPa for as-deposited structures. Such degradations have impact on spectral emissivity, which enhanced upto 0.25 and 0.28 for heat-treated ARTSSCs structures in nitrogen and air ambient, with respect to 0.04 for as-deposited coatings.

B. Usmani, V. Vijay, R. Chhibber, A. Dixit

Chapter 18. A Comprehensive Study of Hydrogen Redistribution and Embrittlement Prevention in Ferrous Alloys

Hydrogen may cause severe degradation on some high strength alloys, and due to their technological and economic relevance, research efforts have intensified in recent years to improve our understanding of such phenomena. A physical model of interstitial element diffusion has been used to study the fluxes of hydrogen during manufacturing of metallic alloys. In particular, the present model contemplates diffusion in its most comprehensive description, i.e. atom diffusion is driven by the gradient in chemical activation, instead of simply occurring down the composition gradients. The model incorporates the influence of thermal history, microstructure, matrix solubility, multiple trapping distributions, and interaction with the atmosphere. This model is able to describe and predict the behaviour of hydrogen during standard industrial practices, and it has been used to explain the effect of component size, cooling rate, microstructure, deformation level, dislocation distribution, grain size, carbide presence and distribution, phase transformation temperature, baking conditions, etc. on hydrogen redistribution. Furthermore, by estimating possible supersaturation at specific regions in the component, it allows to anticipate defect formation and embrittlement risk (and therefore, to prevent them). Not only that, but by using this model, a method has been developed which enables to reduce hydrogen content from the metal via the use of imposed temperature gradients. This method has recently obtained several patents.

Daniel Gaude-Fugarolas

Chapter 19. Advances in Small Specimen Testing Methods for Characterizing Tensile, Creep, and Fracture Properties of Materials

Tensile, impact, and creep properties of materials are evaluated using standard test methods following ISO, ASTM, and other international testing standards. These testing methods use large specimens and are material-intensive. Three innovative small specimen testing methods, namely impression creep (IC), small punch creep (SPC), and ball indentation (BI), are discussed that can be used to determine the mechanical properties of materials. IC is used to study the creep deformation behaviour of materials. SPC is used to evaluate creep deformation and fracture properties of materials. Tensile and hardness properties and fracture toughness can be evaluated using BI method. Unlike in conventional testing methods, all these small specimen testing methods involve complex stresses which are also heterogeneous. Therefore, there is a certain amount of empiricism while characterizing mechanical properties using these methods. However, being material non-intensive, these methods have applications and advantages over conventional methods namely in material development, material performance evaluation, and characterization of mechanical properties of weld joints. This paper presents a comprehensive review of the recent advances in IC, SPC, and BI testing techniques and discusses their relative advantages and limitations.

M. D. Mathew

Chapter 20. An Approach to Develop Hansel–Spittel Constitutive Equation during Ingot Breakdown Operation of Low Alloy Steels

The control of the final quality of a forged product requires an in-depth comprehension of quality of the initial casted ingot. Hot workability is an important property which can be evaluated by variation of strain, strain rate, and temperature. Modeling of forging process always needs to define constitutive models for the material involved. In this study, 42CrMo steel with dendritic microstructure was used to generate the flow stress curves. In order to provide accurate predictions of the thermal and mechanical parameters in the actual ingot break down operation, hot compression tests were carried out at uniform temperatures ranging from 1050 to 1200 °C and strain rates of 0.25–2 s−1. Finally, Hansel–Spittel law was developed to represent the dependency of the material flow stress on strain, strain rate, and temperature. FE Simulation results reveal that the model is able to predict the adiabatic heating during deformation.

K. Chadha, D. Shahriari, M. Jahazi

Chapter 21. Development of an Artificial Neural Network Model for CO2 Corrosion Prediction

Carbon dioxide corrosion (CO2) is responsible for a third of all corrosion-related failures in the oil and gas industry. Due to the fact that there are too many environmental and metallurgical factors with complex interactions, it has been difficult to effectively and accurately predict the rate of CO2 corrosion in any given situation. This work utilises artificial neural network (ANN) techniques to develop a model that can predict CO2 corrosion rates. An experimental and field database of CO2 corrosion of carbon steel was collated, analysed and then used to develop the model. Significance of the selected parameters influencing CO2 corrosion in the oil and gas industry was evaluated using principal component analysis. The final ANN model achieved a correlation coefficient of 0.964 with an accuracy of ±1.6 mm. A graphical user interface was also developed for the model to allow its deployment for further study of CO2 corrosion.

Jacinta Kelly, Krishnan Kannoorpatti, Wai Kean Yap

Chapter 22. Study on the Adhesive Joint Strength of 2060-T8 Al–Li Alloy Single Lap Joint with Different Adhesives

Bonding structures using in the new civil aircraft Al–Li alloy have to possess the characteristics of high safety, long service life, high fatigue strength, and good damage tolerance, which lead to a higher requirements for adhesive selection. Three kinds of typical adhesives were preliminarily selected according to requirements of 2060-T8 Al–Li alloy bonding structure. They are WD1001G, EA9394, and Permabond 910. The strengths of the adhesive joints with these adhesives were, respectively, evaluated with single lap shear (SLS) tests. The appropriate adhesive and the surface morphology in the Al–Li alloy bonding structure were selected. The shear strength of 29.9 ± 0.6 MPa was achieved on surfaces using WD1001G. The maximum shear strength can only reach 5% of the base material tensile strength. Shear strength of 18.2 ± 1.8 and 5.7 ± 1.6 MPa was achieved on surfaces using EA9394 and Permabond 910. Cohesive failure occurred in all the adhesive joints after the SLS tests. Wherein, adhesive failure mainly happened in the adhesive joints using WD1001G and EA9394 as well as interface failure mainly happened in the adhesive joints using Permabond 910.

Xiaohong Zhan, Cheng Gu, Hongliang Wu, Hongbing Liu, Jie Chen, Jicheng Chen, Yanhong Wei

Chapter 23. Mechanical Properties of Ti2AlNb and Ti2AlZr Intermetallics: A First Principles Study

The first principles density function theory (DFT) within generalized gradient approximation (GGA) has been utilized to explain the structural stability and mechanical properties of the of Ti2AlNb and Ti2AlZr intermetallics. The structures of these intermetallics are similar to B2, D019 and O phases. The calculated equilibrium constants for the above phases match very well with experimentally reported values. The D019 and O phases in Ti2AlNb display nearly close value of formation energy/atom. In contrast, formation energy/atom of the B2 phase in Ti2AlNb is lower than that of D019 and O phases. This shows that D019 and O phases are more stable than B2 phase. The decreasing order of formation energy/atom in Ti2AlZr is B2, D019 and O phases. The stability criteria in terms of elastic constants reflect that all the three phases in both the intermetallics are stable. The G/B ratios of all the three phases in both the intermetallics indicate that these phases are ductile. In addition, anisotropy is also present in all the three phases. Interestingly, the degree of anisotropy is significantly high for highest symmetry B2 phase.

Ashish Pathak, A. K. Singh

Chapter 24. Effects of Micro-Ti Addition on Improving Hot Ductility of Nb-Bearing Ultra High Strength Steels

Hot ductility of the continuous casting slabs of new generation of Nb-bearing steels (Ti-added steel #1 and Ti-free steel #2) has been studied using a Gleeble-3500 thermo-mechanical simulator. The influence of micro-Ti on hot ductility and the enhancing mechanism are investigated using OM, SEM and TEM. It is found that the brittle zone III is over the temperature range of 750–900 °C with a minimum reduction in area (RA) of 41.4% at 800 °C for steel #1, and of 650–950 °C with a minimum RA 19.4% at 750 °C for steel #2, respectively. Both steels have brittle zone III; however, the ductility trough of steel #2 is much deeper and wider than that of steel #1, which is mainly related to the film-like ferrite formation at the austenite grain boundaries. TEM morphology confirms Nb(C, N) precipitates at grain boundaries for steel #2. The precipitated particles strongly increase the crack sensitivity of the slab and result in hot ductility deterioration. In contrast, only (Ti, Nb)(C, N) particles are observed inside the grain for steel #1. Ti addition of 0.015 wt% can effectively promote (Ti, Nb)(C, N) to be nucleated on the prior TiN particles. The addition can greatly reduce the negative effect of grain boundary Nb(C, N) precipitations on hot ductility and significantly improve the hot ductility of the steel, thus making steel #1 has a much better hot workability than steel #2. Adding micro-Ti to Nb-bearing steel is an effective way to improve the hot ductility of the new generation of Nb-bearing steels.

Mei Zhang, Haiyang Li, Bin Gan, Chaobin Huang, Hongtao Li, Yong Zhong, Lin Li

Chapter 25. Effect of Transition Metals on Thermal Stability of Al‒Si Cast Alloys

Micro-additions of the transition metals Ti, Zr and V were explored to improve thermal stability of the cast hypoeutectic Al‒7Si‒1Cu‒0.5Mg (wt%) alloy. During high temperature exposures, the Cu- and Mg-rich phases along with the eutectic Si dissolved in the temperature range from 300 to 500 °C whereas the (AlSi)x(TiVZr) phases, containing transition metals, were present until alloy melting. Micro‒additions of Ti, V and Zr increased the alloy strength during testing under both static and cyclic loads. Improvements in the tensile and compressive strength as compared to the reference alloy were observed up to temperatures over 200 °C with more positive effect seen for the T6 state.

F. Czerwinski, S. K. Shaha, W. Kasprzak, J. Friedman, D. L. Chen

Chapter 26. Structure and Properties of the Skeleton Microporous Materials with Coatings Inside the Pores for Medical and Dental Applications

The investigations discussed in the article concern the creation of a new generation of original hybrid microporous high-strength engineering materials ensuring the development of original hybrid constructions of a new generation of personalised implant-scaffolds and tissue scaffolds. The most important is to develop an original hybrid technology of fabrication of a new generation of custom implant-scaffolds and tissue scaffolds using skeleton titanium or Ti6AlV4 alloy microporous materials manufactured by selective laser sintering (SLS). They exhibit porosity and the related mechanical properties dependent on the manufacturing conditions, including mainly laser power, laser beam diameter and distance between laser beams and distance between laser remelting paths. In order to ensure conditions for the nesting and proliferation of living tissues in the micropores of the created porous microskeletons, tests were performed of the deposition of the internal surface of micropores with TiO2 and Al2O3 layers by ALD technology supporting the growth of living tissues in a microporous bonding zone with scaffolds or implant-scaffolds created from engineering materials.

L. A. Dobrzański, A. D. Dobrzańska-Danikiewicz, A. Achtelik-Franczak, M. Szindler

Chapter 27. TWIP Mechanism in High-Mn Austenitic Steels and Its Effect on Steels Properties

The objective of this paper is to define the high-Mn austenitic steels susceptibility to twinning induced by the cold working and influence of it on microstructure and mechanical and plastic properties, and primarily the strain energy per unit volume of newly developed high-Mn austenitic TWIP (Twinning Induced Plasticity)-type steel which contains about 25% of Mn; 1% of Si and 3% of Al. TWIP steels not only present excellent strength, but also have outstanding formability due to twinning, through leading to an exceptional combination of strength, ductility and formability over conventional dual-phase steels. The essence of the investigation concerns the analysis of the importance of microstructure evolution during plastic deformation in ambient temperature. The microstructure of investigated high-Mn steel was determined in metallographic studies using optical microscope and also scanning and high-resolution transmission electron microscopes (HRTEM). Results achieved under static conditions for newly developed advanced high-Mn steel show the opportunity and purposefulness of their use for constructional elements of a body car, especially of the cars’ passenger to take advantage of the meaningful growth of their strain energy per unit volume. It can guarantee a reserve of plasticity in the specially constructed zones and thereby control energy absorption during a potential car accident by activation of twinning induced by cold working. It can also lead to significant growth of the passive safety of those cars’ passengers.

L. A. Dobrzański, W. Borek, J. Mazurkiewicz

Chapter 28. Impact Behaviour of Super Duplex Stainless Steel Weldments at Sub-Zero Temperatures

SAF 2507® is a super duplex stainless steel (SDSS), widely used in highly corrosive environments where high strength is required, for example in offshore and chemical industries. It is known that SDSS below room temperature exhibits a ductile-to-brittle transition in fracture behaviour. The present study is aimed at understanding this behaviour in SDSS weldments using instrumented impact toughness testing. Testing was performed between the room temperature and liquid nitrogen temperature (−196 °C) on the base metal, tungsten inert gas welding (TIG) and submerged arc welding (SAW) material. Results showed that there is a significant difference in the ductile-to-brittle transition temperature (DBTT) between the base metal and the weld metal. In base metal, DBTT was observed to be about −75 °C, −105 °C in TIG weld metal and −55 °C in SAW weld metal. This shows that the DBTT is lowered for the TIG weld metal than compared to the base metal and SAW weld metal due to finer distribution of austenite in the microstructure. The possible reasons for the change in fracture behaviour are discussed.

Raghuveer Gaddam, Guocai Chai, Peter Stenvall

Chapter 29. Microstructural Evolution and Strengthening of Stainless Steels During Cold Rolling

The deformation microstructures and mechanical properties of 304L and 316L stainless steels subjected to caliber cold rolling were studied. The steels were processed by caliber rolling to various total strains from 0.4 to 4.0 at ambient temperature. The structural changes were associated with the development of deformation twinning and partial martensitic transformation. The latter was frequently observed at deformation microbands and deformation twins. The 304L steel samples exhibited faster increase in the fraction of strain-induced martensite during cold rolling as compared to the 316L steel samples. At large strains, the deformation microstructures in the both steels consisted of mixture of highly elongated martensite and austenite crystallites. The cold rolling was accompanied by an increase in the dislocation densities and significant strengthening of the samples. After rolling to a total strain of 4, the yield strengths of 2115 and 1825 MPa were attained in the 304L and 316L steel samples, respectively.

A. Belyakov, M. Odnobokova, A. Kipelova, K. Tsuzaki, R. Kaibyshev

Chapter 30. Influence of Nickel on the Properties of P91 Flux Cored Wire Weld Metal

The creep strength enhanced steel P91 has been used in thermal power plants since the 1990s. As flux cored wires for gas metal arc welding offer several technical and economic advantages, they become more and more popular and also matching flux cored wires for welding P91 have been available for several years. Nickel is often added to filler metals to increase the toughness of the weld metal at room temperature. However, the requirement of Mn + Ni < 1.0 wt% forced the modification of the flux cored wire weld metal. In this contribution, the influence of reduced Ni-content on the mechanical properties at ambient temperature and on creep properties is presented. It confirms that an elevated Ni-content is not necessary to meet the toughness requirements of AWS A5.36.

S. Baumgartner, A. Holy, M. Schuler, R. Schnitzer, N. Enzinger

Chapter 31. Effect of Cross-Linking Agent on the Thermo-Mechanical Properties of Acrylate Shape Memory Polymer Network

Shape memory polymers (SMPs) are currently popular in engineering morphing structures and biomedical applications. In this work, we have synthesized a biodegradable SMP based on poly(ethylene glycol) dimethacrylate (PEGDMA550) as cross-linker, in which tert (butyl acrylate) (tBA) is incorporated as comonomer. The SMP is polymerized by photopolymerization reaction. Further, the macromechanical and thermal properties of the developed SMP are evaluated. Tensile tests have shown that increasing weight content of cross-linker has reduced the elastic modulus significantly. SM properties are characterized by various methods, such as elevated temperature tensile experiments, cyclic thermal mechanical tests, and physical shape recovery tests.

G. Jerald Maria Antony, S. T. Aruna, Raja Samikkannu, Chetan S. Jarali

Chapter 32. Exchange Bias and Interfacial Magnetic Phenomena in Mechanically Milled Ferromagnetic/Antiferromagnetic Nanocomposites

Nanocomposites comprising of ferromagnetic (FM) α-Fe and antiferromagnetic (AFM) MnO, CoO and NiO have been synthesized by high-energy ball-milling for 30 h at 300 rpm speed. Powder X-ray diffraction and Rietveld refinement analysis are used for the microstructural analysis of the samples. Mössbauer spectroscopy shows different relaxation phenomena that indicate polydispersity nature of the samples. Magnetic hysteresis measurements confirm an enhancement in coercivity as well as exchange field. Irreversibility in temperature-dependent magnetization measurement points toward the formation of super-spin-glass-like state arising from wide size distribution of particles. This assumption is confirmed by field-cooled memory effect and temperature cycling in zero-field-cooled magnetization.

Satya Prakash Pati, Dipankar Das

Chapter 33. Effect of Alloying Additions on the Properties Affecting Shape Memory Properties of Cu–12.5Al–5Mn Alloy

The paper discusses the attempt made to understand the role of different alloying additions (Fe, Ni, Cr and Ti) to a Cu–12.5Al–5Mn alloy known to exhibit shape memory behaviour on its microstructure, phase precipitation and effect on transition temperatures after optimising the heat treatment cycles to precipitate the required martensite phase. The effect of the additions has been studied on the optimising conditions, phases precipitated through microstructural analysis‚ X-ray diffraction and transformation temperatures through Differential Scanning Calorimetric studies. In this study, the samples were prepared through liquid metallurgy route by melting pure metals. The cast alloys were subject to homogenisation treatment at 200 °C for 2 h in a muffle furnace and furnace cooled. In an attempt to precipitate the maximum amount of the desired microstructure of martensite in the quenched samples, the quenching cycle was optimised for each alloy by holding them for different duration of time from 30 to 120 min at 920 °C followed by ice quenching. X-ray diffraction studies carried out on the quenched samples indicate martensitic phase precipitation; however, in some cases, the precipitation is incomplete. Differential Scanning Calorimetric (DSC) studies carried out on quenched samples indicate clear transformation peaks in all the samples which are significantly higher than conventionally reported. The range of phase retention was used to determine the enthalpy and entropy changes. The findings confirm the possibility of changing the shape memory properties such as martensite formation, transitions temperatures, retention times, thermal properties as in entropy and enthalpy change with changing alloying constituents. Attempts have been made to study the shape memory properties of selected alloys that have exhibited promising improvement over the base alloy. The study can help pinpoint compositions with the desired properties in such alloy systems.

Rupa Dasgupta, Ashish Kumar Jain, Shahadat Hussain, Abhishek Pandey, V. Sampath

Chapter 34. Characterization of Fine Metal Powders Produced by Hybrid by Water–Gas Atomization for Metal Injection Molding

The effects of water pressure on the particular size, oxygen content, tap density, and yield by hybrid by water–gas atomization were described in this paper. 316L stainless steel has been atomized successfully with this technique. Median diameters (D50) of powder by laser diffraction method are between 8 and 13 μm, the tap density of the powder exceeds 4.7 g/cm3, and the particle shape observed by scanning electron microscope (SEM) is spherical.

Zhu Jie, Luo Hao, Weng Ting, Li Zhi, Zong Wei, Zeng Keli


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