用球形单晶体研究干涉色与晶体位向的关系

通过对工业纯铁的球形单晶体试样化学染色，全方位地显示了各种位向表面的干涉色及各干涉色在球面上的对称分布特征，经Ｘ射线背射芳厄法位向分析标定出各干涉色与晶体位向的对应关系，绘制出相位化染图案的单位赤面投影三角形，结果表明，单晶体金属表面上的每一种干涉色对应于一定范围内的许多不同位向。球面化染图案具有与被染色金属晶体的结构桢的对称性，可用于晶体的定量测定。     

Correlation between grain orientation and the shade of color etching

Color etching is an extremely effective metallographic technique not only for making grains well visible, but also for making them distinguishable for automated image analyzers. During color etching, a thin film is formed on the surface of the specimen. The thickness of this layer is in the order of magnitude of the visible light and since both the metal-film boundary and the film surface reflect light, an interference occurs. A wavelength-component of the white line is eliminated and its complementary color will be seen on the surface. As the thickness changes, the colors also change grain by grain.The thickness of the film is dependent on several factors, mostly on the type of the phase. However, different color shades can be observed on the surfaces of single phase materials, which phenomenon is caused by the different crystallographic orientations of the grains.This paper shows a combined color etching electron backscatter diffraction (EBSD) investigation of cast iron. An area of the surface of a gray cast iron specimen was etched. Colors were characterized by their luminescence and their red, green and blue intensity. An EBSD orientation map was taken from the same area and the orientations of the individual grains were determined.Results showed that a strong correlation was found between the luminescence and the R, G, B intensity of the color and the angle between the specimen normal and the < 100> direction, while such correlation was not observed between the color parameters and the < 110 > and < 111> directions, respectively. This indicates that film thickness is sensitive to the < 100> direction of the crystal.     

Direct evidence of advantage of Cu(111) for graphene synthesis by using Raman mapping and electron backscatter diffraction

The advantageous crystallographic orientation of Cu surface for graphene synthesis by using thermal chemical vapor deposition (CVD) is examined by Raman mapping and electron backscatter diffraction. It is found that Cu(111) predominates over (110) and (100) for single- (SLG) or few-layer graphene (FLG) growth. To confirm this result we attempt the synthesis of graphene on Cu(111) single crystal film surfaces. We confirmed the formation of high quality and high uniformity SLG or FLG over more than 97% of the substrate surface area of 10 mm × 10 mm by Raman mapping.     

Grain boundary and fracture surface analysis of Fe–C–P steel

Abstract

The present paper investigates the distribution of grain boundary types and fracture surface crystallography in an Fe–C–P alloy. It is shown that electron backscatter diffraction (EBSD) is an effective technique with which to conduct these investigations. The proportions of both Σ1 and particularly Σ3 (in coincidence site lattice notation)present after various heat treatments were higher than would have been expected for random generation. There was limited evidence that both higher annealing temperatures and longer annealing times promoted generation of Σ3 type boundaries. The standard EBSD technique was modified and extended to encompass both the novel ‘matched fracture’ specimen approach and direct mapping from fracture surfaces to provide crystallographic information. A correlation was noted between higher aging temperatures and proportions of cleavage fracture. Furthermore, there was a strong correlation between cleavage fracture surfaces exhibiting river markings and an {001} surface orientation.     

Determination of crystallographic orientation of dwell-fatigue fracture facets in Ti-6242 alloy

A technique to determine the crystallographic orientation of the fracture facets has been described. The spatial orientation of the facet plane is determined in a scanning electron microscope (SEM) using a quantitative tilt fractography technique. The crystallographic orientation of the grain, across which a particular fracture facet had been produced, is determined using the electron backscattered diffraction (EBSD) technique in an SEM. These two pieces of information were combined to obtain the crystallographic orientation of the fracture facet normal. This technique was used for the characterization of dwell-fatigue fracture facets at the crack-initiation site in Ti-6242 alloy. Our results indicate that these facets are not exactly aligned with the basal plane, but are inclined at ∼10° to it.     

Effect of Crystallographic Anisotropy on Micro EDM Process

In this paper, experiments are conducted by machining from different crystallographic orientations of monocrystalline silicon, and the effects of crystallographic orientation on the micro electrical discharge machining (EDM) process are discussed. The results demonstrate that the machining speed and surface roughness are varied when crystallographic orientation changes. The surface roughness is seen to vary by as much as twofold with crystallographic orientation, while the ratio between the maximum and minimum values of material removal rate is 1.76. The unique material removal mechanism of micro EDM enhances the effects of crystal anisotropy on micro electrical discharge machining process.     

Variable‐Wavelength Quick Scanning Nanofocused X‐Ray Microscopy for In Situ Strain and Tilt Mapping

Compression of micropillars is followed in situ by a quick nanofocused X‐ray scanning microscopy technique combined with 3D reciprocal space mapping. Compared to other attempts using X‐ray nanobeams, it avoids any motion or vibration that would lead to a destruction of the sample. The technique consists of scanning both the energy of the incident nanofocused X‐ray beam and the in‐plane translations of the focusing optics along the X‐ray beam. Here, the approach by imaging the strain and lattice orientation of Si micropillars and their pedestals during in situ compression is demonstrated. Varying the energy of the incident beam instead of rocking the sample and mapping the focusing optics instead of moving the sample supplies a vibration‐free measurement of the reciprocal space maps without removal of the mechanical load. The maps of strain and lattice orientation are in good agreement with the ones recorded by ordinary rocking‐curve scans. Variable‐wavelength quick scanning X‐ray microscopy opens the route for in situ strain and tilt mapping toward more diverse and complex materials environments, especially where sample manipulation is difficult.     

Crystallographic analysis of plate martensite in Fe–28.5 at.% Ni by FE-SEM/EBSD

Crystallographic analysis of plate martensite in an Fe–28.5 at.% Ni alloy was studied by electron backscattering diffraction (EBSD) in a scanning electron microscope equipped with a field emission gun (FE-SEM). It was shown that sound orientation mapping was possible even for the martensite having a high density of lattice defects and the FE-SEM/EBSD could be a strong tool for crystallographic/microstructural analysis of martensite in steels. It was confirmed that the martensite in this alloy held the Nishiyama–Wassermann (N–W) orientation relationship. Variant analysis of every martensite crystal was successfully done from orientation mapping data. It was clarified that a certain rule of variant selection operated within local areas. The procedures of crystallographic analysis of N–W martensite were explained in detail.     

A study of nucleation, growth, texture and phase formation of electrodeposited cobalt layers and the influence of magnetic fields

Cobalt (Co) layers with a thickness of up to 50 nm have been electrodeposited under the influence of magnetic fields up to 10 T aligned perpendicular or parallel to the electrode surface. The crystallographic orientation and the phase composition of these layers have been investigated by X-ray diffraction and transmission electron microscopy. The layers consist mainly of the face centered cubic phase with a 〈111〉 orientation perpendicular to the electrode surface which results from the low surface free energy of these planes. An influence of magnetic fields on the crystallographic orientation has not been observed. It was found that magnetic fields affect the phase composition which results predominantly from the influence of the magnetic fields on the electrochemistry. The nucleation has been studied by in-situ scanning tunneling microscopy.     

Sharp DNA bends as landmarks of protein-binding sites on straightened DNA

We have developed a fluorescence-based method for mapping single or multiple protein-binding sites on straightened, large-size DNA molecules (> 5 kbp). In the described method, protein-DNA complexes were straightened and immobilized on a flat surface using surface tension. A fraction of the immobilized complexes displayed a sharp DNA bend with two DNA segments extending from the apex. The presence of DNA-binding proteins at the apex was verified by atomic force microscopy. The position of protein binding relative to the ends of the DNA molecule was determined by measuring the length of two DNA segments using fluorescence microscopy. We demonstrate the potential of the fluorescence-based method to localize protein-binding sites on the DNA template and to evaluate relative binding affinity. The proposed protein-binding-site mapping technique is simple and easy to perform. Practical applications include screening for DNA-binding proteins and the localization of protein-binding sites on large segments of DNA.     

Two-dimensional versus three-dimensional post-deposition grain growth in epitaxial oxide thin films: Influence of the substrate surface roughness

Epitaxial thin films made of nanosized yttria-stabilized zirconia islands deposited on (0001) sapphire substrates are synthesized by sol-gel dip-coating followed by a high-temperature post-deposition thermal annealing procedure. At high temperatures, a competitive growth process takes place that allows to obtain thin films made of atomically flat islands with an in-plane diameter typically ten times higher than the thickness or on the contrary inducing the formation of dome-shaped islands. Apart from having a different shape, these islands are also characterized by a different crystallographic orientation with respect to the substrates respectively (001) and (111). In this paper, we investigate the influence of the substrate surface roughness on this competitive grain growth process. The deposition on epi-polished substrates results in a two-dimensional (2D) island growth, whereas the deposition on rough substrates results in a three-dimensional (3D) growth of dome-shaped nanosized islands. The films have been characterized by atomic force microscopy and high-resolution X-ray diffraction using the reciprocal space mapping technique.     

Step motion of the growth surface in the initial stage of semiconductor film epitaxy with ion sputtering

The development of relief inhomogeneity of the surrounding surface near (111)Si by thermal heating in an UHV oil pumped and gettered system has been studied. The essential features of the surface relief are discussed in connection with pre-epitaxial preparation of the substrate surface used for growing Si films by sputtering. The initial growth stage of layers 25, 65, 240 and 480 Å thick at a substrate temperature of 840°C is illustrated.It is shown that the formation of growth macrosteps is due to a complex system of sites for adatoms on the original Si surface because of the presence of etch micropits and silicon carbide particles. The conditions for formation of a crystallographic system of microsteps (with height of atomic order) on Si surfaces in the absence of etch pits and silicon carbide particles are analysed. The adsorption parameters and surface diffusion coefficient of adatoms are estimated.     

Crystallographic alignment of calcite prisms in the oblique prismatic layer of Mytilus edulis shell

The structure and crystallographic orientation of mineral phase in the oblique prismatic layer of Mytilus edulis shell were studied by SEM, XRD and TEM with selected area electron diffraction (SAED). A crystallographic orientation regulation, i.e. the adjacent 1–5 calcite prisms with the same three-dimensional orientation in the oblique prismatic layer, was found for the first time. It is observed that the calcite prisms in the oblique prismatic layer were grown with their (104) parallel to the shell surface.     

Antibacterial activity of ZnO powder with crystallographic orientation

ZnO powder with crystallographic orientation was prepared from the mixed aqueous solution of zinc chloride, tri-ethanol amine and thio-urea. From X-ray diffraction measurement, as-prepared powder was found to have the orientation along a–b axes of hexagonal structure, and a needle-like shape with the aspect ratio of 5 was observed by scanning electron microscope, indicating that as-prepared powder had crystallographic orientation. In the tests of antibacterial activity by colony count method, ZnO powders with and without crystallographic orientation were used in present work. Survival ratio of bacteria decreased with increasing powder concentration, i.e., increase in antibacterial activity. The antibacterial activity in ZnO powder with crystallographic orientation was weaker than that in commercial ZnO powder without orientation at same powder concentration. Regarding specific surface area of the powders used in antibacterial tests, however, antibacterial activity in powder with orientation was found to be similar to that without orientation; that is, the crystallographic orientation of ZnO did not affect antibacterial activity. The activity toward Staphylococcus aureus was stronger than that toward Escherichia coli, irrespective of the kind of powders.     

Molecular dynamics simulation of incipient plasticity of nickel substrates of different surface orientations during nanoindentation

The present study aims to elucidate the anisotropic characteristics in material responses for crystallographic nickel substrates with (001), (011) and (111) surface orientations during nanoindentation. Molecular dynamic simulation is applied to compensate for the experimental limitation of nanoindentation, particularly for pure nickel substrates. Defect nucleation and evolution in Ni single crystal of these three crystal orientations was examined. Hardness and Young’s modulus are also extracted in different orientations. The Young’s modulus of (111) crystallographic orientation is the largest, while that of (001) surface is the smallest. The sensitivity of the yield point for face centred cubic crystals depends on the crystallographic orientation. The (001) crystallographic orientation reaches the yield point first, while the (111) crystallographic orientation is the most difficult in which to achieve yield. Using a visualisation method of centrosymmetry parameter, the homogeneous nucleation and early evolution of dislocations were investigated, deepening understanding of incipient plasticity at the atomic scale. The present results suggest that defect nucleation and evolution are the root of curve jitter. The indentation depth of the elastic–plastic transition point varies in the different crystallographic orientation models, and appears latest in the (111) model. The strain energy of the substrate exerted by the tip is stored by the formation of homogeneous nucleation and is dissipated by the dislocation slide in the {111} glide plane. The three nickel substrates with different crystallographic orientations exhibit different forms of dislocation propagation.     

Acicular ferrite nucleation and growth in API5L-X65 steel submerged arc welded joints

In the present study, acicular ferrite nucleation and growth were investigated from a crystallographic point of view in API5L-X65 steel weld metals. It was observed that acicular ferrite was nucleated on inclusions in weld metal. The titanium-enriched layer around inclusions was characterised as the TiO phase by selected area diffraction patterns. A scanning electron microscope equipped with an electron backscatter diffraction technique was applied to investigate the crystallographic orientation relationship. The results showed that acicular ferrite lathes had a Baker–Nutting orientation relationship with the TiO layer on the inclusion surface in the nucleation of acicular ferrite. However, it is confirmed that the growth of acicular ferrite lathes depends on the deviation from the Kurdjumov–Sachs relationship between lathes and primary austenite.     

Texture development in cold rolled and annealed C-Mn-Si and C-Mn-Al-Si TRIP steels

Abstract

The texture of two transformation induced plasticity steels has been studied by means of crystallographic orientation mapping. Texture measurements were carried out on ferrite, bainite, and austenite. The polygonal ferrite and the bainite texture, both bcc, could be distinguished based on the image quality parameter of the electron backscattering diffraction measurement. Both bcc textures were very similar, the main difference being the more pronounced 111alpha ND ND=normal direction and 110alpha RD RD=rolling direction fibre textures in the polygonal ferrite. The fcc texture was a strong gamma deformation texture, characterised by the beta fibre. The presence of the alpha fibre confirmed the strong 110gamma ND direction, which was previously detected by means of X ray diffraction XRD. The measured fcc and bcc textures were used to calculate orientation distribution function transformations according the Bain, Kurdjumov-Sachs, and Nishiyama-Wasserman orientation relationships. The predicted cube component {001}gamma 100gamma, which was missing in the measured texture, of gammaret indicates a variant selection for the gammaalphaB transformation. In addition it was shown that crystallographic orientation mapping could be used to make reliable phase fraction determinations, which were previously based on the light optical microscopy of colour etched specimens. This also proves that XRD determination of gammaret is flawed owing to the strong texturing of all phases present in the microstructure.     

Effects of sputtering pressure and nitrogen concentration on the preferred orientation of AIN thin films

Aluminium-nitride films were prepared on glass substrates by reactive radio frequency (r.f.) magnetron sputtering in argon/nitrogen gas mixtures containing 25 ~ 75 1/2; nitrogen at substrate temperatures below 150C. It is important to control the crystallographic orientation and the surface morphology of the films with the deposition parameters for surface-acoustic-wave (SAW) devices. The change of crystallographic orientation with the sputtering pressure and the nitrogen concentration was calculated from the texture coefficient of the (0002) plane based on X-ray diffraction (XRD) patterns. It was found that a change of the c-axis from a parallel to a normal orientation, with respect to the substrate surface, occurred with a decrease in the sputtering pressure and an increase in the nitrogen concentration. From observations of the cross-section and the surface morphology, aluminium-nitride films exhibited a columnar structure and the grain size at the film surface increased an increase in the sputtering pressure and with a decrease in the nitrogen concentration.     

Cover Picture: Large‐Area 3D Nanostructures with Octagonal Quasicrystalline Symmetry via Phase‐Mask Lithography (Adv. Mater. 10/2007)

A novel method for producing large‐area 3D nanostructured quasicrystalline materials uses 2D multiple exposure lithography to produce an octagonal quasiperiodic surface‐relief template (background image). A replica in polydimethylsiloxane is then used as a phase mask to create 3D bicontinuous axial quasicrystalline SU‐8 epoxy nanostructures (see insets), as reported on p. 1403 by Ion Bita, Edwin Thomas, and co‐workers.