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Short crack propagation under cyclic loading is compared experimentally in hydrogen charged and un-charged SA508 Gr. 3 Cl. I low alloy steel (LAS). This LAS is used in manufacturing of pressure vessels installed in nuclear power plants and is susceptible to hydrogen embrittlement (HE) during operation. Single edge notch tension (SENT) specimens with an initial notch of 85 μm–90 μm are used for this short fatigue crack propagation study. The short crack growth from the notch of SENT specimen subjected to cyclic loading is measured using moving digital microscope fitted on the servo-hydraulic fatigue testing machine. The short fatigue crack growth rate in hydrogen charged SA508 Gr. 3 Cl. I LAS is found to be one order higher as compared to the un-charged subject reactor pressure vessel (RPV) steel. Both trans-granular and inter-granular crack propagation is observed in un-charged and hydrogen charged specimens. In un-charged specimens, inter-granular crack propagation along the prior austenite grain boundaries (PAGBs) occurred only when the short fatigue crack encounters the martensite/austenite (M/A) island present along the PAGB. Whereas, in hydrogen charged specimens, inter-granular crack propagation occurred along the PAGBs of large size prior austenite grains and trans-granular crack propagation through the small size prior austenite grains. Strong resistance to short fatigue crack propagation is provided by PAGBs in un-charged specimens whereas, these PAGBs offered negligible resistance to short fatigue crack growth in hydrogen charged subject RPV steel. A new perspective of studying HE in materials by conducting short fatigue crack growth experiments is demonstrated.

Correlating hydrogen embrittlement phenomenon with the metallic microstructural features holds the key for developing metals resistant to hydrogen-based failures. In case of fatigue failure of hydrogen charged metals, in addition to the hydrogen-based failure mechanisms associated with monotonic loading such as HELP, HEDE etc., microstructural features such as grain size, type of grain boundary (special/random), fraction of special grain boundaries; their network and triple junctions can play a complex role. The probable sites for fatigue crack initiation in such metals can be identified as the sites of highest hydrogen concentration or accumulated plastic strain. To this end, we have developed an experimental framework based on in-situ fatigue crack initiation and propagation studies under scanning electron microscope (SEM) to identify the weakest link in the metallic microstructure leading to failure. In-situ fatigue experiments are performed on carefully designed polycrystalline nickel (99.95% pure) specimens (miniaturised, shallow-notched & electro-polished) using a 10 kN fatigue stage inside the SEM. Electron Back Scattering Diffraction (EBSD) map of the notched region surface helps identify the distribution of special/random grain boundaries, triple junctions and grain orientation. The specimen surface in the shallow notched region for both the hydrogen charged and un-charged specimens are then carefully studied to correlate the microstructural feature associated with fatigue crack initiation sites. Such correlation of the fatigue crack initiation site and microstructural feature is further corroborated with the knowledge of hydrogen trapping and grain’s elastic anisotropicity to be either the site of high hydrogen concentration, accumulated plastic slip or both.

Hydrogen Embrittlement (HE) leads to deterioration of the fracto-mechanical properties of metals. In spite of vast literature, it is still not clearly understood and demands significant research on this topic. For better understanding of the hydrogen effect on fatigue behaviour of metals, present work focuses on developing a computational framework for fatigue crack initiation studies in metals in the presence of hydrogen. The developed framework consists of a nonlocal crystal plasticity model coupled with hydrogen transport model to study the fatigue behaviour of hydrogen charged metals. The nonlocal crystal plasticity model accounts for the statistically stored dislocations (SSDs) and geometrically necessary dislocations (GNDs) in polycrytalline metal. Hydrogen transport model, on the other hand, accounts for diffusion and trapping behavior of hydrogen due to concentration gradient, pressure gradient, plastic strain-rate with dislocations as the only trapping sites along the slip systems. A polycrystalline representative volume element (RVE) with periodic boundary conditions is used in this study. Fatigue crack initiation criterion is proposed for the simulated RVE with controlled microstructure by considering a critical value of the fatigue indicator parameter (FIP). FIP is formulated based on the experimental observations of several crack initiation sites along the grain boundaries, their normal direction with respect to loading direction and the accumulated plastic strain in nickel polycrystalline samples. Developed simulation framework correctly accounts cyclic stress-strain behavior and multiple fatigue crack initiation sites observed experimentally in the presence of hydrogen.

The effect of hydrogen on short crack propagation under cyclic loading in SA508 Grade 3 Class I low alloy steel is investigated. This low alloy steel is used in manufacturing of pressure vessel installed in Indian nuclear power plants. During operation these pressure vessels are subjected to continuous supply of pressurized hot water at 600 K and hence are susceptible to hydrogen embrittlement. In past, research has been conducted on the effect of hydrogen embrittlement on long fatigue crack propagation in this material but, the mechanistic understanding and correlation of hydrogen embrittlement with microstructural features in the material can be understood well by studying the effect of hydrogen embrittlement on short fatigue crack propagation. Short fatigue cracks are of the order of 10 µm to 1 mm and unlike long cracks these short cracks strongly interact with the microstructural features in the material such as grain/phase boundaries. The effect of hydrogen embrittlement on short crack propagation is studied by artificial hydrogen charging of the material through electrochemical process. The single edge notch tension (SENT) specimens with an initial notch of the order of 85 to 90 µm are used to study the short crack propagation. The short cracks in hydrogen charged samples initiated from the notch at lower number of loading cycles as compared to the uncharged notched samples for the same value of applied stress range (Δσ). After initiation, the short fatigue crack in hydrogen charged samples propagated at higher rate as compared to uncharged samples. This dissimilarity in crack propagation behavior is due to the difference in the interaction of short fatigue crack with the microstructural features for a hydrogen charged and uncharged samples.

Histidine is an essential α-amino acid that plays a crucial role in tissue development and helps in the transmission of metallic ions during biological events. However, an abnormal level of histidine in the body is associated with various physiological conditions such as arthritis, liver cirrhosis, kidney diseases, and asthma. Herein, a unique ratiometric fluorescence sensing system has been developed for the recognition of histidine. The sensing system was developed using carbon quantum dots (CQDs) as an energy donor and a rhodamine 6G derivative (HS30) as an energy acceptor unit. Interestingly, upon the addition of Fe(III) into the mixture of CQDs and HS30, the phenomenon of fluorescence resonance energy transfer (FRET) was observed when excited at 350 nm. The emergence of a strong emission peak at 551 nm on the addition of Fe(III) suggested the formation of a ratiometric fluorescent complex “CQDs–Fe–HS30”. The ratiometric behavior of “CQDs–Fe–HS30” was studied by monitoring fluorescence emissions at 425 nm and 551 nm with an excitation wavelength of 350 nm. Furthermore, “CQDs–Fe–HS30” was employed for the recognition of histidine in an aqueous system. Due to the high affinity of histidine to Fe(III), the addition of histidine to an aqueous solution of “CQDs–Fe–HS30” resulted in the displacement of the Fe(III) cation from the complex, and the simultaneous quenching and enhancement of the emission peaks at 551 nm and 425 nm, respectively, was observed. The developed sensing system was successfully employed for a histidine recovery experiment in human urine samples with satisfactory results. Furthermore, the mixture of CQDs and HS30 was successfully utilized to implement an inhibit logic gate with Fe(III) and histidine as inputs and emission at 551 nm as output.

Understanding hydrogen embrittlement phenomenon that leads to deterioration of mechanical properties of metallic components is vital for applications involving hydrogen environment. Among these, understanding the influence of hydrogen on the fatigue behaviour of metals is of great interest. Total fatigue life of a material can be divided into fatigue crack initiation and fatigue crack growth phase. While fatigue crack initiation can be linked with the propagation of short fatigue cracks, the size of which is of the order of grain size (few tens of microns), that are generally not detectable by conventional crack detection techniques applicable for the long fatigue crack growth behaviour using conventional CT specimens. Extensive literature is available on hydrogen effect on long fatigue crack growth behaviour of metals that leads to the change in crack growth rate and the threshold stress intensity factor range (ΔKth). However, it is the short fatigue crack growth behaviour that provides the fundamental understanding and correlation of the metallic microstructure with hydrogen embrittlement phenomenon. Short fatigue crack growth behaviour is characteristically different from long crack growth behaviour showing high propagation rate at much lower values than threshold stress intensity factor range as well as a strong dependency on the microstructural features such as grain boundaries, phase boundaries, and inclusions. To this end, a novel experimental framework is developed to investigate the short fatigue crack behaviour of hydrogen charged materials involving in-situ observation of propagating short cracks coupled with image processing to obtain their da/dN vs a curves. Various metallic materials ranging from austenitic stainless steel (AISI 316L) to reactor pressure vessel steel (SA508 Grade 3 Class I low alloy steel) and line pipe steels (API 5L X65 & X80) are studied in this work.

Aim of the paper is to understand the effect of microstructural features of SA508 Grade 3 Class I low alloy steel (LAS) on short crack propagation rate under cyclic loading. The complex upper bainitic microstructure of this LAS consists of low angle bainitic ferrite lath boundaries and high angle prior austenite grain boundaries (PAGBs). Compared to bainitic ferrite lath boundaries, the PAGBs provided major hindrance to short fatigue crack propagation in the subject LAS. The high angle PAGBs strongly resist the dislocation motion ahead of the crack tip as the crack tip approaches the PAGBs compared to that of low angle bainitic ferrite lath boundaries. This restriction of dislocation motion ahead of the crack tip based on hindrance provided by PAGBs resulted in retardation in short fatigue crack propagation rate along the crack path. The short fatigue crack propagated at stress intensity factor (SIF) range ‘ Δ K ’ values lower than threshold SIF range ‘ Δ K t h ’ for the long cracks. The growth rate of short fatigue cracks cannot be predicted by Paris law which is applicable for long crack growth. This is due to the fact that crack growth rate undergoes acceleration and retardation in short crack regime because of microstructural effects.

From thick to very thin specimens, fracture toughness of metallic materials peaks out before hitting much lower value compared to the constant plane strain fracture toughness value obtained using standard fracture mechanics testing of thick specimens. Understanding this behavior is essential for improving reliability of small-scale metallic devices currently being used for various critical applications. To understand this behavior, it is essential to study the process of dislocations emission and interaction at the crack front and its variation with specimen thickness. To this end, atomistic fracture simulations of pre-cracked single crystal FCC metal (Nickel) specimens representing both thick and thin specimens are performed. At first, stress-state dependent single crystal yield function based on the generalized Schmid-law is associated with the dislocation emission process at the crack front for both thin and thick specimens. Fracture simulations are then performed on single crystal specimens representing different thickness cases. Due to low stress triaxiality prevailing throughout the thickness of thin specimens, dislocation interaction with each other inside the specimen and then with the specimen surface leading to wedge-shaped groove formation on opposite surfaces at crack front is found to be the responsible mechanism of crack propagation in thin specimens. This mechanism provides enhanced fracture toughness to thin specimen compared to thick specimen in which crack propagation is based on high stress triaxiality at the core of the crack front making formation of microvoids and their coalescence as a dominant mechanism of crack propagation. The dislocation configurations generated at the crack front for thick and thin specimens are also studied and the mechanisms for dislocation multiplication in thin specimens compared to thick specimens are highlighted.

Molecular dynamics (MD) simulations offer an interesting route to simulating deformation and fracture behavior of amorphous glassy polymers. However, MD simulations are performed at extremely high rates and on very small samples (though periodic boundary conditions are routinely used) containing at most hundreds of chains which are much shorter than in real life. In this work, we try to assess the extent to which MD simulations produce physically realistic stress–strain responses and identify aspects of the simulation procedure that can be controlled closely in order to avoid numerical artifacts. We show that, when an appropriate protocol for sample generation and simulation of deformation is followed, in spite of the obvious constraints imposed by the simulation technique, MD simulations have the capability to generate realistic stress–strain curves and reproduce many experimental trends pertaining to them.

Short fatigue cracks, having dimension less than 1 mm, propagate at much faster rates (da/dN) even at lower stress intensity factor range (da/dN) as compared to the threshold stress intensity factor range obtained from long fatigue crack growth studies. These short cracks originate at the sub-grain level and some of them ultimately transit into critical long cracks over time. Therefore, designing the components subjected to fatigue loading merely on the long crack growth data and neglecting the short crack growth behavior can overestimate the component’s life. This aspect of short fatigue cracks become even more critical for materials used for safety critical applications such as reactor pressure vessel (RPV) steel in nuclear plants. In this work, the transition behaviour of short fatigue crack gowth into long fatigue crack is studied in SA508 Grade 3 Class I low alloy steel used in RPVs. In-situ characterization of initiation, propagation and transition of short fatigue cracks is performed using fatigue stage for Scanning Electron Microscope (SEM) in addition to digital microscopes fitted over a servo-hydraulic fatigue machine and correlated with the microtructural information obtained using electron backscatter diffraction (EBSD). SA508 steel having an upper bainitic microstructure have several microstructural interfaces such as phase and grain boundaries that play a significant role in controlling the short fatigue crack propagation. Specially designed and prepared short fatigue specimens (eletro-polished) with varying initial crack lengths of the order of tens of microns are used in this study. The transition of such short initial cracks into long cracks is then tracked to give detailed insight into the role of each phase and phase/grain boundary with an objective of establishing Kitagawa-Takahashi diagram for the given RPV steel. The behavior of the transited long cracks is then compared with the crack propagation behavior obtained using conventional CT specimens. The outcome of this research will enhance information on the integrity of the components made from RPV steel used in Indian nuclear power plants.

The primary objective of this work is to model the growth and eventual failure of a craze fibril in a classy polymer, starting from a primitive fibril. Experimental investigations have shown that properties like the entanglement density of a polymer play a pivotal role in determining whether macroscopic failure of a polymer occurs through crazing or shear yielding. Failure is seen to be related to the formation of a soft 'active zone' at the craze-bulk interface. through disentanglement. The present work aims at explaining some of the experimental findings about fibril growth and failure in glassy polymers on the basis of a continuum model of a craze with a constitutive model that accounts for yield, network hardening and disentanglement. The results show that this approach is capable of providing explanations for experimentally observed facts such as the propensity to crazing in polymers with low entanglement density and the linearity between the stretch in a fibril and the maximum stretch of a molecular strand in the fibril. (c) 2005 Elsevier Ltd. All rights reserved.