Crystallographic orientation dependence of nanoindentation hardness in austenitic phase of stainless steel

ABSTRACT

This paper presents the indentation hardness evolution in different in-plane directions of austenite grains whose {111} planes are parallel to the sample surface determined by nanoindentation tests and electron back scattering diffraction (EBSD) analysis. A scanning electron microscopy (SEM) image of the indentation surface around one of the indents indicated the activation of two sets of slip planes with respect to each of the three indenter surfaces for a Berkovich tip. The identification of the slip traces by EBSD data analysis is in accord with Schmid`s law. We therefore proposed a new approach for defining the orientation parameter to interpret the indentation hardness. The orientation parameter was shown to be the minimum value of the three maximum Schmid factors on the secondarily activated slip planes in three directions for a Berkovich tip. Indentation hardness increased with the decrease in the orientation parameter and was dependent on in-plane orientation.     

Plasticity of GaAs(011) at room temperature under concentrated load

Indentations have been made on a (011) surface of GaAs single crystal at room temperature. The loading-unloading curves were compared with those obtained under the same experimental conditions on (001) surfaces. The indents formed were observed by transmission electron microscopy in plan view as well as in cross-sectional view in samples prepared by the focused-ion-beam technique. The gliding systems could be identified, providing a better understanding of the plastic flow under the indenter. The arrangements of dislocations generated by the indenter have been analysed and compared with results previously reported by Ning et al.     

High-resolution electron microscopy observations of microplastic fracture in SiC under ball milling at room temperature

Nanometre-sized kinks and cracks formed in 6H SiC under ball milling (BM) at room temperature have been observed and characterized on the atomic scale using high-resolution electron microscopy (HREM). Observations of the kinks show that numerous positive and negative partials are aligned at either of the kink boundaries, and the stacking sequences in the kink band are considerably different from those in the other areas. It was also observed that the (0001) lattice planes in the kink band are kinked, indicating that microplasticity occurs in the normally brittle material SiC under BM even at room temperature. HREM observations of cracks show that cracks previously observed by transmision electron microscopy are not completely open but are at the initiation stage of fracture. Inside a crack, one residual kink region can be clearly observed, which indicates a correlation between kink and crack, that is a crack evolves from a kink.     

Transmission electron microscopy observations of low-load indents in GaAs

Nanoindentations have been made on (001) surfaces of GaAs single crystals at room temperature and the indents observed by transmission electron microscopy. The permanent deformation, generated by a Berkovitch indentor submitted to maximum loads ranging between 600 to 1700 muN, was analysed and interpreted as a function of the loading curves. The plastic zone size was measured as a function of the maximum load to determine the yield strength of GaAs at room temperature. Finally, the fine structure of the dislocations generated by the indenter has been analysed and this is compared with previously reported structures for higher indenting loads.     

Microstructure evolution and hardness variation of pack-rolled nanocrystalline nickel

The microstructure evolution and hardness of nanocrystalline nickel during pack rolling at room temperature have been investigated. It was found that the roll-bonding side (R) and non-roll-bonding side (NR) behaved quite differently. The hardness of side R is higher than that of side NR. No obvious work softening was observed in either side R or side NR until the strain reached ~ 0.611. Quantitative X-ray diffraction analysis indicated that the grain size in side NR increases faster than that in side R, a result confirmed by transmission electron microscopy. Texture analysis showed that (2 0 0) preferred orientation first strengthens but then weakens in both sides NR and R, while a strong (2 2 0) preferred orientation emerges, particularly in side R. Further texture analysis suggests that dislocation slip is responsible for the texture discrepancy between side NR and side R. The dislocation activity, grain rotation and grain growth are discussed based on the experimental results.     

Plastic behaviour of an AlAs/GaAs superlattice with a short period

Nanoindentation has been used to investigate the plastic behaviour of an AlAs/GaAs superlattice with a short period. The sample was grown on a (001) surface of a GaAs single crystal by metal-organic vapour-phase epitaxy. The mechanical response of the superlattice to nanoindentation testing was compared with that of a (001) surface of bulk GaAs. The indents formed were observed by transmission electron microscopy. The plastic zone size associated with each indent was measured as a function of the maximum load. Finally the arrangement of the dislocations generated by the indenter has been analysed and compared with the arrangement observed in deformed bulk GaAs.     

Growth orientation of one-dimensional silicon nanowires prepared by thermal evaporation

One-dimensional silicon nanowires have been grown by thermal evaporation and their growth orientations determined by transmission electron microscopy studies. The nanowires, which are often highly curved in morphology and heavily twinned in microstructure, are crystallographically separated into several sections, each with a characteristic crystallographic orientation along the wire axis. Straight nanowires, or straight sections in a curved nanowire, are found to have non-unique crystallographic orientations when {111} twinning occurs.     

TEM observation of the restrained Goss–Brass orientation transformation in a warm-rolled Fe–28Mn–6Si–5Cr shape memory alloy

A dominant Goss texture component instead of a Brass texture component has been observed in a warm-rolled Fe–28Mn–6Si–5Cr shape memory alloy [H. Li, F. Yin, T. Sawaguchi K. Ogawa, X. Zhao and K. Tsuzaki, Mater. Sci. Eng. A 494 (2008) p.217]. In order to clarify the orientation flow mechanism in these grains of Goss orientation, investigations on microtexture and microstructure were carried out by electron backscattering diffraction (EBSD) and transmission electron microscopy (TEM). It is concluded that the Goss–Brass orientation transformation is restrained in the Goss-orientated grains, which were widely observed in both the deformed matrix and shear bands.     

Fragmentation testing for ductile thin films on polymer substrates

Fragmentation testing of thin films on substrates has in the past been mostly performed in situ using optical and scanning electron microscopy. While these techniques work well for brittle materials, they cannot always discern the difference between through-thickness cracks (TTCs) and localized plastic deformation of ductile films. Here, we describe fragmentation testing with atomic force microscopy and present criterion to distinguish TTCs and localized deformation for ductile films.     

In situ transformation from P phase to μ phase in rhenium-containing single-crystal superalloy during thermal exposure

An in situ phase transformation from P to μ in a rhenium-containing superalloy during high-temperature exposure has been investigated by transmission electron microscopy. The orientation relationship between the phases is found as (1–12)_μ // (1?0?0)_P and [2?4?1]_μ // [0?1?1]_P. An atomic model of the μ/P interface was built to reveal a perfectly coherent interface with lattice misfits of only 0.421 and 1.098%. Considering the small lattice distortions and the similar elemental composition of the phases, it is concluded that the phase transformation from P to μ is favourable.     

Aluminium precipitates in the primary silicon of as-sprayformed hypereutectic aluminium-silicon alloys

Precipitates have been observed in the primary silicon of as-spray-formed hypereutectic aluminium-silicon alloys with and without various alloy additions. The precipitates have been investigated using transmission electron microscopy and high-resolution transmission electron microscopy. They are aluminium based and generally adopt a spheroidal morphology, with diameters in the range of approximately 5-10nm, unless located on a stacking fault or grain boundary. Spray forming is a rapid solidification process and precipitation occurs because of the low solid solubility of aluminium in silicon (maximum of 0.016 +/- 0.003at.% at 1190 C). The morphology of the precipitates suggests that they form from aluminium or aluminium-rich liquid. The orientation relationships of several precipitates in one of the primary silicon grains have been determined.     

Debonding criterion for the piezoelectric fibre push-out test

An Al-Ni-Co pentagonal quasicrystal, showing electron diffraction patterns with pentagonal symmetry and including so-called superlattice reflections, has been examined by the high-angle annular detector dark-field technique with scanning transmission electron microscopy. Columnar clusters with a pentagonal arrangement of transition-metal atoms around their centres are arrayed in a rhombic tiling with a bond length of 2nm, all the clusters having the same orientation of pentagonal symmetry.     

Amorphization under fracture surface in hydrogen-charged and low- temperature tensile-tested austenitic stainless steel

ABSTRACT

The microstructure just below the fracture surface in hydrogen-charged stable austenitic SUS 316L stainless steel, which was subjected to a low strain rate tensile test at ?70°C, was studied by a combination of the focused-ion-beam method and transmission electron microscopy. An amorphous region with a chemical composition almost identical to that of the polycrystalline region was found under the lath-like structure on the fracture surface, although no deterioration of tensile properties by hydrogen appeared. In the amorphous region, band-like regions with wavy contrasts were observed, which were often accompanied by cracks at the boundaries. The presence of the amorphous region with band-like regions implies that amorphization occurred due to high-density vacancies accompanied by agglomerations of excess vacancies in the hydrogen-charged SUS 316L stainless steel that was tensile-tested at low temperatures.     

Revealing texture architecture in a surface gradient nanostructured Al-Cu-Mg alloy

ABSTRACT

A multiscale crystallographic texture architecture in a surface gradient nanostructured Al-Cu-Mg alloy after surface sliding friction treatment (SSFT) has been revealed by a combination of electron backscatter diffraction and precession electron diffraction (PED)-assisted transmission electron microscopy (TEM) orientation mapping. Accompanying a grain structure variation from lamellar coarse grains to equiaxed nanograins, the major texture components evolve from brass {110}<112> in the coarse-grain matrix, Goss {110}<001> at a depth of ～80?μm, E {111}<011> and F {111}<112> at a depth of ～20?μm, to a mixture of rotated cube {001}<110>, E and F in the topmost surface layer. The through-thickness textural development and evolution are attributed to the cyclic loading of concurrent shear and compression during the SSFT processing. The PED-assisted orientation mapping shows good capability in mapping severe plastic-deformation-induced nanostructures with large residual strains and high defect density.     

Identification of a new tetragonal phase in the Nb-Ti-Al system

During the course of investigation of the phase equilibria in the Nb-Ti-Al system, a new phase, designated theta, was observed in three Nb-Ti-40at.%Al alloys following ageing at low temperatures (less than 1000 C). Using X-ray diffraction and transmission electron microscopy techniques, this phase was determined to have a bct structure, with lattice parameters a₀ = 5.106 A and c₀ = 28.168A, a space group of I 4₁/amd (number 141) and composition near 45at.%Nb25at.%Ti-30at.%Al. An orientation relationship between the new tetragonal phase and the gamma-TiAl phase of [101]_gamma//[120]_theta and (111)_gamma//(001)_theta was observed within the microstructure.     

Inversion domain boundary in a ZnO film

Transmission electron microscopy has been used to investigate the (1100) and (1103) inversion domain boundaries in a ZnO film prepared by molecular beam epitaxy. The inversion domain was revealed by dark-field images and confirmed by convergent-beam electron diffraction. Interacting with a (0002) stacking fault, the inversion domain boundary in the (1100) plane alters its orientation from the [0001] direction and climbs on the (1103) plane to release the strain energy. These features are characterized and analysed by high-resolution electron microscopy and the geometric phase method. The findings are significant for understanding the formation and propagation of inverse domain boundaries in epitaxial ZnO films.     

Electron back-scatter diffraction study of inoculation of Al

The microstructure of cast commercial-purity aluminium inoculated by addition of an Al-Ti-C grain refiner has been studied by scanning electron microscopy and electron back-scatter diffraction (EBSD). It is found that a small fraction of the TiC particles present in the melt act as nucleation centres for grains. EBSD shows that the aluminium grains have a crystallographic cube-cube orientation relationship with the particles on which they nucleate. Nucleation occurs only on the largest particles, consistent with model predictions. Despite potential thermodynamic instability, TiC particles are effective nucleating agents.     

3D shape and orientation of nanoscale Pb inclusions at grain boundaries in Al observed by TEM and STEM tomography

We have combined high-angle annular dark field/scanning transmission electron microscopy (HAADF-STEM) tomography with bright field (BF)-TEM tomography to characterize small inclusions of Pb at a grain boundary in Al. It was found that the shape of the grain boundary inclusions is more complex than previously thought. By using moiré fringes observed at some orientations of the specimen in a BF-TEM tomographic tilt series, we were able to determine the orientation of each grain, the axis and angle of misorientation of the grain boundary, and the facet planes of the grain boundary inclusions. The 3D shape of the inclusions was determined by merging this information with the HAADF-STEM tomography.     

Grain orientation effects on delamination during fatigue of a sensitized Al–Mg alloy

Fatigue crack growth experiments were conducted in humid air (RH~45%) at 25 °C on 29-mm-thick plate samples of an aluminium–magnesium (Al–Mg) 5083-H131 alloy in the long transverse (LT) direction. Samples were tested in both the as-received condition and after sensitization at 175 °C for 100 h. Delamination along some grain boundaries was observed in the short transverse plane after fatigue testing of the sensitized material, depending upon the level of ΔK and K_max. Orientation microscopy using electron backscattering diffraction and chemical analyses using transmission electron microscopy and energy dispersive spectroscopy of grain boundaries revealed that Mg segregation and the orientation of grains had key roles in the observed grain boundary delamination of the sensitized material.     

Combined effect of strontium modifier and antimony refiner on texture and growth mode of eutectic phase in an Al-11Si-2Cu-0.8Zn-0.6Fe cast alloy

Results of electron back-scattered diffraction and transmission electron microscopy studies reveal that the orientation of aluminium in the eutectic phase is different from the surrounding aluminium dendrites and that twin spacing of eutectic silicon increased significantly due to the interaction between strontium and antimony. In addition, the formation of ternary Mg₂Sb₂Sr intermetallic compound that precedes the eutectic reaction was proposed to be responsible for interaction.