Comparison of microstructures for plane shock-loaded and impact crater-related nickel: the microtwin-microband transition

Plane-wave shock-loaded Ni exhibits {111} microtwins which increase in frequency with increasing peak shock pressure above a critical twinning pressure of 30 GPa. In contrast, microbands coincident with traces of {111} are produced below impact craters in Ni targets by stainless steel projectiles at velocities up to 3.5 km/s. The microband widths are ten times the 0.02 m twin widths and are characterized by misorientations of roughly 2°. Both shock-loaded and impacted Ni have similar dislocation cell structures which decrease in cell size with increasing pressure or equivalent stress. The exclusive formation of microbands in connection with impact craters in Ni is expected on the basis of its high SFE (130 mJ/m²), and a simple dislocation model is developed for the microtwin-microband transition based on graphical summaries which include shock (stress) geometry and SFE effects in FCC metals and alloys.     

Phase transition study of superconducting microstructures

The presented results are part of a feasibility study of superheated superconducting microstructure detectors. The microstructures (dots) were fabricated using thin film patterning techniques with diameters ranging from50µm up to500µm and thickness of1µm. We used arrays and single dots to study the dynamics of the superheating and supercooling phase transitions in a magnetic field parallel to the dot surface. The phase transitions were produced by either varying the applied magnetic field strength at a constant temperature or changing the bath temperature at a constant field. Preliminary results on the dynamics of the phase transitions of arrays and single indium dots will be reported.     

Microstructural transformations in austenitic-ferritic transition joints

The relatively complex microstructures developed at the interface between ferritic steel and weld metal on austenitic-ferritic transition joints have been examined by metallographic observation and by hardness tests in the as-welded condition and in the as-welded-and-tempered condition. Both austenitic stainless steel and nickel-based filler metals were used in welds. On as-welded specimens a sharp change of hardness in low-alloy steel has been measured, with increasing distance from weld metal; the hardness values have been related to the observed metallographic constituents. On post-weld heat treated specimens, the behaviour is different according to the composition of filler material, either austenitic steel or nickel-based alloy. In the case of austenitic filler material, a dark-etching narrow diffusion region of carbon toward weld metal is formed, with an adjacent markedly decarburized zone, exhibiting the minimum microhardness values in a narrow band of about 60 micrometres. Since this sharp structural variation is recorded just in the zone where often failures occur, the final post-weld heat treatment appears to be proposed with due caution. In the case of nickel-based filler material, carbon diffusion is inhibited by the precipitation of alloy carbides at the weld interface. This determines a more homogeneous heat affected zone (HAZ) in the ferritic steel and a reduced decarburization near the fusion line after a post-weld heat treatment, confirming the reasons of the preference recognized to this filler material, especially when service temperature is elevated and submitted to frequent changes, or whenever a post-welded heat treatment is required.     

Characterisation and intrinsic magnetic resonance properties of nickel nanoparticles

Nickel nanoparticles have been extensively characterised by atomic force microscopy (AFM), scanning electron microscopy (SEM) and confocal micro-Raman spectroscopy. AFM underestimates the particle size compared to SEM measurements. It is shown that Raman spectroscopy can detect the nanometre-thick NiO layer on the particles having frequency shifts of the modes indicative of phonon confinement. The magnetic properties of the particles are studied by ferromagnetic resonance (FMR) of magnetic field aligned particles. The alignment is achieved by suspending the particles in the liquid crystal MBBA and freezing the liquid in a 0.4 T DC magnetic field. The in-field solidification locks the direction of maximum magnetisation of the particles parallel to the direction of the applied DC magnetic field. This removes the effects of dynamical particle fluctuations of the nanoparticles on the magnetic properties allowing a study of the intrinsic magnetic properties of the magnetic nanoparticles. The intensity of the FMR signal decreased with lowering temperature for the particles frozen in the liquid in a 0.4 T DC magnetic field. The effect is suggested to be due to a reduction of the microwave skin depth with lowering temperature.     

Characterisation of moisture-dependent cohesive zone properties for adhesively bonded joints

Structural adhesives are being widely used in the aerospace and automobile industries. However, in many applications, aggressive environments damage the adhesive systems and degrade the structural performance of bonded members. Cohesive zone models are often employed in the numerical analysis of adhesively bonded structural joints. To accurately model these bonded joints, the characterisation of the cohesive zone properties for different environmental conditions is important. In this regard, an experimental-numerical approach was developed to characterise the environment-dependent cohesive zone properties based on a miniature cantilever peel test. As moisture is a commonly encountered aggressive environment, the current methodology was implemented to characterise the moisture-dependent cohesive zone properties for an Al 2024-T3 and FM73 system.     

Characterisation of dynamic recrystallisation in nickel using processing map for hot deformation

Abstract

The hot deformation behaviour of polycrystalline nickel has been characterised in the temperature range 750–1200°C and strain rate range 0·0003–100 s^?1 using processing maps developed on the basis of the dynamic materials model. The efficiency of power dissipation, given by [2m/(m+1)], where m is the strain rate sensitivity, is plotted as a function of temperature and strain rate to obtain a processing map. A domain of dynamic recrystallisation has been identified, with a peak efficiency of 31% occurring at 925°C and 1 s^?1. The published results are in agreement with the predictions of the processing map. The variations of efficiency of power dissipation with temperature and strain rate in the dynamic recrystallisation domain are identical to the corresponding variations of hot ductility. The stress–strain curves exhibited a single peak in the dynamic recrystallisation domain, whereas multiple peaks and ‘drooping’ stress–strain curves were observed at lower and higher strain rates, respectively. The results are explained on the basis of a simple model which considers dynamic recrystallisation in terms of rates of interface formation (nucleation) and migration (growth). It is shown that dynamic recrystallisation in nickel is controlled by the rate of nucleation, which is slower than the rate of migration. The rate of nucleation itself depends on the process of thermal recovery by climb, which in turn depends on self-diffusion.

MST/1524     

Characterisation of hot isostatically pressed nickel base superalloy Inconel* 718

Abstract

Inert gas atomised Inconel 718 superalloy powder was characterised for various important properties and subsequently consolidated by hot isostatic pressing (hipping) at 1200° C and 120 MPa for 3 h. The density of the as compacted material was nearly the same as its theoretical density. Optical microscopy of as hipped material showed a fine grained structure with no porosity but having annealing twins and prior particle boundaries (PPBs). Electron probe microanalysis (EPMA) studies revealed that the PPBs were decorated with Al, Ti oxides, and MC type carbides enriched with Nb and Ti. In addition to these phases, the presence of very fine γ"-Ni₃Nb and γ'-Ni₃(Al,Ti) precipitates in the matrix were revealed by TEM analysis, which indicates that the compacted material was partially aged during the slow cooling stage of hipping. Tensile tests conducted on the as hipped material showed that the ultimate tensile strength (UTS) and ductility values were comparable to those obtained in the (solution treated and two step aged) wrought alloy 718, although its yield strength was marginally lower at room temperature.     

Characterisation of oxide scales formed on nickel superalloy using impedance spectroscopy

Abstract

Impedance spectroscopy has been used to measure the electrical properties of oxide scales formed from oxidation of IN738LC superalloy at high temperature. Electrical resistance and capacitance of the oxide scales were obtained from the simulation of the measured impedance diagrams based on the equivalent circuit model, which represents the features of the oxide scales. For oxidation of IN738LC superalloy, the electrical resistance of oxide scales increased with increasing oxidation time for the specimens exposed to air at 900°C. However, for the specimens oxidised at 1,200°C, the oxide scales showed very low electrical resistance, which indicated that cracking and spallation in oxide scales occurred continuously. By using scanning electron microscopy and X-ray diffraction techniques, the composition and microstructure of the oxide scales were examined. It was found that electrical properties were determined, not only by the microstructure of oxide scales, but also by the composition of the oxide scales. By determining the relationship between electrical properties, microstructure and composition of oxide scales, impedance spectroscopy could be used as a non-destructive technique for monitoring the oxidation of metallic alloys at high temperature.     

Structure and properties of diffusion bonded transition joints between commercially pure titanium and type 304 stainless steel using a nickel interlayer

The solid-state diffusion bonding was carried out between commercially pure titanium and Type 304 stainless steel using nickel as an interlayer in the temperature range of 800–900 °C for 9 ks under 3 MPa load in vacuum. The transition joints thus formed were characterized in the optical and scanning electron microscopes. The inter-diffusion of the chemical species across the diffusion interfaces were evaluated by electron probe microanalysis. TiNi₃, TiNi and Ti₂Ni are formed at the nickel–titanium (Ni–Ti) interface; however, the stainless steel–nickel (SS–Ni) diffusion interface is free from intermetallic compounds up to 850 °C temperature. At 900 °C, the Ni–Ti interface exhibits the presence of α-β Ti discrete islands in the matrix of Ti₂Ni and λ + χ + α-Fe, λ + FeTi and λ + FeTi + β-Ti phase mixtures occur at the SS–Ni interface. The occurrence of different intermetallics are confirmed by the x-ray diffraction technique. The maximum tensile strength of ∼276 MPa and shear strength of ∼209 MPa along with 7.3% elongation were obtained for the diffusion couple processed at 850 °C. At the 900 °C joining temperature, the formation of Fe–Ti base intermetallics reduces the bond strength. Evaluation of the fracture surfaces using scanning electron microscopy and energy dispersive spectroscopy demonstrates that failure takes place through Ni–Ti interface up to 850 °C and through the SS–Ni interface of the joint when processed at 900 °C.     

Characterisation of optically driven microstructures for manipulating single DNA molecules under a fluorescence microscope

Optical tweezers are powerful tools for manipulating single DNA molecules using fluorescence microscopy, particularly in nanotechnology‐based DNA analysis. We previously proposed a manipulation technique using microstructures driven by optical tweezers that allows the handling of single giant DNA molecules of millimetre length that cannot be manipulated by conventional techniques. To further develop this technique, the authors characterised the microstructures quantitatively from the view point of fabrication and efficiency of DNA manipulation under a fluorescence microscope. The success rate and precision of the fabrications were evaluated. The results indicate that the microstructures are obtained in an aqueous solution with a precision ∼50 nm at concentrations in the order of 10⁶ particles/ml. The visibility of these microstructures under a fluorescence microscope was also characterised, along with the elucidation of the fabrication parameters needed to fine tune visibility. Manipulating yeast chromosomal DNA molecules with the microstructures illustrated the relationship between the efficiency of manipulation and the geometrical shape of the microstructure. This report provides the guidelines for designing microstructures used in single DNA molecule analysis based on on‐site DNA manipulation, and is expected to broaden the applications of this technique in the future.Inspec keywords: DNA, molecular biophysics, fluorescence, optical microscopy, radiation pressure, biological techniquesOther keywords: optically driven microstructures, single DNA molecule analysis, fluorescence microscopy, optical tweezers, nanotechnology‐based DNA analysis, manipulation technique, aqueous solution, fine tune visibility, yeast chromosomal DNA molecules, geometrical shape, on‐site DNA manipulation     

The toughness of laser welded joints in the ductile-brittle transition

An important feature of laser welded joints is the high level of strength and toughness mismatch developed between the weld and the parent plate. As a result, defects are frequently located in regions with high strength and toughness gradients. To address this issue, toughness tests have been performed on laser welded joints with strength mismatches in excess of 2. Toughness tests have been performed on high and low constraint mode I geometries and mixed-mode I/II configurations. In highly constrained geometries, the local toughness dominates the failure process causing the crack to deviate into harder and more brittle weld metal, while in low constraint configurations, the size of the plastic zone promotes crack deviation into the softer and tougher parent plate. In Charpy tests the crack also deviates into the tougher parent plate giving potentially misleading indications of the behaviour of defects in highly constrained joints. The experiments are modelled by a local approach technique for functionally graded materials in which the local yield strength and toughness are allowed to vary spatially.     

Characterisation of residual stress distribution in clinching joints of carbon steel by diffraction methods

Abstract

Sheet joints of carbon steel fabricated by two different clinching methods, namely TOX and Eckold, have been investigated. The holding force of the joints was determined by shear tension tests and the deformation microstructure was characterised using optical microscopy. The surface residual stress and mean residual stress distributions as a function of increasing distance from the outer diameter of the interlock button were mapped by X-ray and neutron diffractometry, respectively. The Eckold joints showed more severe joint distortion in the form of global sheet bending, but nevertheless possessed higher shear tension strength than the TOX joints. Characteristic residual stress distributions depending on the clinching method were found in both the TOX and Eckold joints. The observed residual stress distributions have been attributed to the different die construction employed by the two methods, which permitted different degrees of plastic deformation during clinching.     

Inconel718合金扩散连接接头的组织与性能研究

对细晶Incone1718高温合金无中间层和加Ni箔中间层两种情况下的扩散连接进行了研究,分析了不同的连接温度、连接压力、连接时间等工艺参数对接头剪切强度的影响;通过SEM、EPMA和金相技术对接头微观组织和力学性能进行了分析.确定了获得优质接头的最佳工艺参数区间,即扩散连接温度T=1 050℃,连接压力P=20 MPa,连接时间t=45 min,选用Ni箔作为中间层,厚度为25 μm.     

Wetting of nickel alloys by nickel based brazes

Abstract

Sessile drop spreading tests have been carried out to evaluate the influence of braze and substrate chromium content on the wetting and flow of Ni–Cr–Si–B and Ni–Cr–P brazes on nickel and Ni–Cr substrates. The effect of filler metal chromium additions is examined in terms of fluidity processes, while the role of base metal chromium content is discussed in the context of oxide reduction and alloying phenomena.

MST/1056     

The effect of processing variables on the microstructures and properties of aluminum brazed joints

Aluminum brazed joints are used extensively in the automotive and aircraft industries. In order to insure the integrity of the bond, the effects of processing variables on the quality of the bond must be understood. The effects of brazing period and joint thickness on the microstructure, tensile properties, microhardness and micromechanisms of failure of two aluminum alloy 3003 plates connected by a layer of 4047 aluminum filler material were investigated. It was found that the amount of aluminum-silicon eutectic microstructure in the reaction zone decreased with increasing brazing period and decreasing joint thickness. This was attributed to silicon diffusion from the joint material and dissolution of base metal and its entrance into the liquid joint. The amount of shrinkage porosity in the reaction zone was found to increase with increasing brazing period due to base material solutioning. The ultimate tensile strength of joints decreased with increasing brazing period and decreasing joint thickness. This was attributed to the joint microstructure and shrinkage porosity formed in the joint. Shrinkage porosity was found to be the primary cause of decreased joint strength. Joints with 10 minutes brazing period failed within the base material, while for brazing periods greater than 10 minutes, joints failed within the aluminum-silicon eutectic microstructure of the reaction zone. This indicated that the joint strength was greater than the base material for joint with brazing period of 10 minutes. Finite element analysis was performed to determine the effect of joint material yield strength and joint thickness on the stress and strain field in the brazed joint. Finite element analysis results supported experimental observations.     

Fatigue failure transition analysis in load‐carrying cruciform welded joints based on strain energy density approach

This paper details a study of the application of notch stress intensity theory to the fatigue failure mode analysis of the transition in load‐carrying cruciform welded joints. The weldment fatigue crack initiation point is difficult to predict precisely because it usually occurs in the vicinity of the weld toe or weld root. To investigate the relationship between fatigue failure location and the geometry of the weldments, we analysed the weld toe and root asymptotic notch stress fields were analysed using the notch stress intensity factors on the basis of the Williams' solution in Linear Elastic Fracture Mechanics (LEFM). Numerous configurations of cruciform joints of various plate thicknesses, transverse plate thickness, weld sizes and incomplete penetration size were used to investigate the location of the fatigue failure. The strain energy density (SED) surrounding the notch tip was introduced to unify the scalar quantity and preclude the inconsistency of the dimensionality of the notch stress intensity factors for various notch opening angles. The results of the investigation showed that the SED approach can be used to determine the transition zone for a variety of joint geometries. The validity of the SED criteria was verified by comparing the experimental results of this study with the complied results for load‐carrying cruciform welded joints reported in literature.     

The electrical and magnetic properties of the transition in nickel sulfide

The Hall effect and resistivity have been measured on single crystals of hexagonal NiS above and below the transition temperature, and magnetic susceptibility measurements have been made on powders and ground-up single crystals in the same temperature region. It is found that the material behaves as an extrinsic semiconductor in the low temperature region, with the charge carriers arising from the nickel vacancies.     

Creep rupture properties of nickel-base transition joints after long-term service

Abstract

Three superheater transition joints, between 2·25Cr–1 Mo and 316 stainless steel, welded with nickel–base weld metal, removed from service after 72337 h, have been examined using optical and scanning electron microscopy. In addition, microhardness measurements have been made and local chemical compositions have been analysed using the energy dispersive X-ray attachment on a scanning electron microscope. Temperature accelerated creep rupture tests have been carried out between 590 and 625°C at stresses of 31–62 MN m^?2 on cross–weld tensile specimens machined longitudinally from the walls of the joints. Detailed metallographic examinations showed the same failure mode as that found in long–term service failures. Therefore, the use of post-exposure temperature accelerated testing of uniaxial cross-weld specimens appears to be a viable method of assessing the remanent life of nickel-base transition joints operating at elevated temperatures. The applicability of various multiaxial stress rupture equations to transition joint failures is considered. The present rupture data are compared with previous data generated from initially as-welded specimens to provide upper and lower estimates of the long-term failure lives.

MST/403     

Variation of fractographic appearance for different microstructures in welded joints having the same fatigue crack propagation properties

Fatigue fracture surfaces were examined with a scanning electron microscope to investigate the influence of the different microstructure between weld metal and heat affected zone. The specimens were centre-cracked type transverse butt welded joints. The relationship between macroscopic fatigue crack propagation rate and the stress intensity factor range is the same in spite of the difference in microstructure for both materials. It is shown that the fractographic appearance changes with microstructure even in the very low growth rate region near fatigue threshold. This suggests that fractographic appearance is not necessarily a guide to the rate of fatigue crack growth.