Backscattered electron imaging and electron backscattered diffraction in the study of bacterial attachment to titanium alloy structure

The application of secondary electron (SE) imaging, backscattered electron imaging (BSE) and electron backscattered diffraction (EBSD) was investigated in this work to study the bacterial adhesion and proliferation on a commercially pure titanium (cp Ti) and a Ti6Al4V alloy (Ti 64) with respect to substrate microstructure and chemical composition. Adherence of Gram‐positive Staphylococcus epidermidis 11047 and Streptococcus sanguinis GW2, and Gram‐negative Serratia sp. NCIMB 40259 and Escherichia coli 10418 was compared on cp Ti, Ti 64, pure aluminium (Al) and vanadium (V). The substrate microstructure and the bacterial distribution on these metals were characterised using SE, BSE and EBSD imaging. It was observed that titanium alloy‐phase structure, grain boundaries and grain orientation did not influence bacterial adherence or proliferation at microscale. Adherence of all four strains was similar on cp Ti and Ti 64 surfaces whilst inhibited on pure Al. This work establishes a nondestructive and straight‐forward statistical method to analyse the relationship between microbial distribution and metal alloy structure.     

A study of recrystallization in single-phase aluminium using in-situ annealing in the scanning electron microscope

In‐situ annealing experiments were performed in the scanning electron microscope on a single‐phase Al?0.13Mg alloy cold rolled to different strain levels. Once the validity of the technique had been verified by comparison of the recrystallization kinetics and final grain size with bulk annealed samples, the method was used in combination with electron back‐scattered diffraction (EBSD) to study the potential mechanisms for recrystallization in this alloy. During annealing of material rolled to moderate strains (?_t < 0.7), the primary mechanism was strain‐induced boundary migration (SIBM). In material rolled to higher true strains (?_t > 1.4), recrystallization occurred extensively along pre‐existing cube bands and EBSD measurements showed that the mean size of cells within the cube bands was larger than for all other orientations measured, suggesting a size advantage was responsible for the strengthening of cube texture during recrystallization. SIBM was shown to occur concurrently with the nucleation along cube bands but this contributed a lower proportion of nucleation sites during recrystallization.     

Recrystallization phenomena in an IF steel observed by in situ EBSD experiments

In situ electron backscatter diffraction microstructural analysis of recrystallizing interstitial free steels deformed to strains of 0.75 and 1.6 has been carried out in a FEG‐SEM. The experimental procedures are discussed, and it is shown that there is no degradation of the electron backscatter diffraction patterns at temperatures up to 800°C. Analysis of the surface and interior microstructures of annealed samples shows only minor difference, which suggests that in situ annealing experiments are of value. In addition, it is shown that in situ measurements allow a detailed comparison between the same areas before and after annealing, thereby providing information about the recrystallization mechanisms. Sequential recrystallization phenomena, such as initiation and growth of new grains, are observed at temperatures over 740°C, and depending on the deformation histories, different recrystallization behaviour is observed. It is found that {111}〈123〉 recrystallized grains are preferentially formed in the highly deformed material, whereas no strong recrystallization texture is formed in the lower strained material.     

Study of dynamic grain growth by electron microscopy and EBSD

The effect of hot deformation on fully recrystallized aluminium–copper alloys (Al-4wt%Cu and Al-33wt%Cu) with different volume fractions of CuAl₂ has been studied. The alloys are Zener pinned systems with different superplastic properties. Strain-induced grain growth, observed in both alloys, was quantitatively estimated by means of electron microscopy and EBSD and compared with the rate of static grain growth. Surface marker observations and in situ hot-deformation experiments combined with EBSD were aimed at clarifying the mechanisms responsible for the changes in the deformed microstructures. A sequence of secondary and backscattered electron images and EBSD maps was obtained during in situ SEM deformation with different testing conditions. Overlaying EBSD maps for the Al-4wt%Cu with channelling contrast images showed that grain boundary motion occurred during deformation, creating a layered structure and leading to an increase in size of some grains and shrinkage of others. Of a particular interest are results related to behaviour of CuAl₂ in superplastic Al-33wt%Cu during deformation, including several problems with the use of EBSD in this alloy.     

The structure and mechanical properties of amorphous and nanocrystalline Fe–Si–B alloys

This article describes the results of investigations of the microstructure of failure surfaces and the mechanism of deformation of an amorphous Fe₈₀Si₁₁B₉ alloy, nanocrystallized with the use of Nd:YAG pulsed laser heating. The research included ‘in situ’ tensile testing in a scanning electron microscope. Mechanical properties were also measured on an Instron‐type machine for the amorphous and nanocrystalline alloys. The mechanical tensile tests performed on the amorphous and nanocrystalline samples showed a ductile fracture surface with very high fracture stress. Detailed observations of the flow deformation and fractures revealed the relationship between the quenched‐in crystalline and mechanical behaviour.     

Quasi-cleavage fracture planes in spheroidized A533B steel

Electron backscattered diffraction (EBSD) has been used to acquire crystal orientation information around unusual microcracks induced by tensile deformation of notched specimens of spheroidized A533B steel. This unusual fracture mode has been called quasi‐cleavage and occurs at relatively low temperatures with fracture energies below that of the upper shelf. EBSD measurements on sectioned samples showed that the quasi‐cleavage cracks were intragranular. A two‐dimensional analysis technique was used in which EBSD measured crystal orientations were combined with secondary electron imaging to obtain the trace of the crack facet on the section plane. The measurements revealed that the observed crack facets were consistent with crack propagation along the {001} and {011} planes.     

User‐independent EBSD parameters to study the progress of recovery and recrystallization in Cu–Zn alloy during in situ heating

Microstructural evolution of cold‐rolled Cu–5%Zn alloy during in situ heating inside field‐emission scanning electron microscope was utilized to obtain user‐independent parameters in order to trace the progress of static recovery and recrystallization. Electron back‐scattered diffraction (EBSD)‐based orientation imaging microscopy was used to obtain micrographs at various stages of in situ heating. It is shown that unlike the pre‐existing methods, additional EBSD‐based parameter can be used to trace the progress of recovery and recrystallization, which is not dependent on user input and hence less prone to error. True strain of 0.3 was imposed during cold rolling of alloy sample. Rolled sample was subjected to in situ heating from room temperature to 500°C (～0.58 Tm) with soaking time of 10 min, at each of the intermediate temperatures viz. 100, 200, 300, 400 and 450°C. After reaching 500°C, the sample was kept at this temperature for a maximum duration of around 15 h. The sample showed clear signs of recovery for temperature up to 450°C, and at 500°C, recrystallization started to take place. Recrystallization kinetics was moderate, and full recrystallization was achieved in approximately 120 min. We found that EBSD parameter, namely, band contrast intensity can be used as an extra handle to map out the progress of recrystallization occurring in the sample. By contrast, mean angular deviation can be used to understand the evolution of recovery in samples. The parameters mentioned in the current study, unlike other pre‐existing methods, can also be used for mapping local microstructural transformations due to recovery and recrystallization. We discuss the benefits and limitations in using these additional handles in understanding the changes taking place in the material during in situ heating.     

Characterization of nitride thin films by electron backscatter diffraction

Thin films incorporating GaN, InGaN and AlGaN are presently arousing considerable excitement because of their suitability for UV and visible light‐emitting diodes and laser diodes. However, because of the lattice mismatch between presently used substrates and epitaxial nitride thin films, the films are of variable quality. In this paper we describe our preliminary studies of nitride thin films using electron backscattered diffraction (EBSD). We show that the EBSD technique may be used to reveal the relative orientation of an epitaxial thin film with respect to its substrate (a 90° rotation between a GaN epitaxial thin film and its sapphire substrate is observed) and to determine its tilt (a GaN thin film was found to be tilted by 13 ± 1° towards [101 0]_GaN), where the tilt is due to the inclination of the sapphire substrate (cut off‐axis by 10° from (0001)_sapphire towards (101 0)_sapphire). We compare EBSD patterns obtained from As‐doped GaN films grown by plasma‐assisted molecular beam epitaxy (PA‐MBE) with low and high As₄ flux, respectively. Higher As₄ flux results in sharper, better defined patterns, this observation is consistent with the improved surface morphology observed in AFM studies. Finally, we show that more detail can be discerned in EBSD patterns from GaN thin films when samples are cooled.     

Sample preparation and microscopical investigation techniques for metal and ceramics containing graphite and graphene‐like layered particles

Scanning electron microscopy (SEM) techniques are widely used in microstructural investigations of materials since it can provide surface morphology, topography, and chemical information. However, it is important to use correct imaging and sample preparation techniques to reveal the microstructures of materials composed of components with different polishing characteristics such as grey cast iron, graphene platelets (GPLs)‐added SiAlON composite, SiC and B₄C ceramics containing graphite or graphene‐like layered particles. In this study, all microstructural details of gray cast iron were successfully revealed by using argon ion beam milling as an alternative to the standard sample preparation method for cast irons, that is, mechanical polishing followed by chemical etching. The in‐lens secondary electron (I‐L‐SE) image was clearly displayed on the surface details of the graphites that could not be revealed by backscattered electron (BSE) and Everhart–Thornley secondary electron (E‐T SE) images. Mechanical polishing leads to pull‐out of GPLs from SiAlON surface, whereas argon ion beam milling preserved the GPLs and resulted in smooth surface. Grain and grain boundaries of polycrystalline SiC and B₄C were easily revealed by using I‐L SE image in the SEM after only mechanical polishing without any etching process. While the BSE and E‐T SE images did not clearly show the residual graphites in the microstructure, their distribution in the B₄C matrix was fully revealed in the I‐L SE image.     

Orientation averaging of electron backscattered diffraction data

The use of data averaging to improve the angular precision of electron backscattered diffraction (EBSD) maps is discussed. It is shown that orientations may be conveniently and rapidly averaged using the four Euler-symmetric parameters which are coefficients of a quaternion representation. The processing of EBSD data requires the use of an edge preserving filter and a modified Kuwahara filter has been successfully implemented and tested. Three passes of such a filter have been shown to reduce orientation noise by a factor of ∼10. Application of the method to deformed and recovered aluminium alloys has shown that such data processing enables small subgrain misorientation (< 0.5°) to be detected reliably.     

A preliminary electron backscattered diffraction study of sintered NdFeB-type magnets

This paper reports, for the first time, the use of electron backscattered diffraction (EBSD) to study orientation in sintered NdFeB type magnets. The magnetic properties of NdFeB magnets are greatly improved if a strong crystallographic texture is firstly achieved, namely, the direction of the c‐axis is along the direction of magnetization. A systematic survey of sample preparation techniques showed that samples that were mechanically polished and then etched gave the most reliable EBSD data. Analyses were made using both fully automated EBSD scans and by EBSD measurements taken after manual movement of the beam. The EBSD results are presented as secondary electron SEM micrographs, orientation images and 001 pole figures. For the selection of grains investigated, the deviation of the c‐axis was shown to be between 10° and 30° from the ideal [001]//magnetization direction. It is demonstrated that EBSD is a valuable tool for characterizing the microstructure and texture relationships and for assessing the performance of the processing routes of NdFeB magnets.     

Crystallographic orientation of ZrB2-ZrC composites manufactured by the spark plasma sintering method

The crystallographic grain orientation of ZrB₂‐ZrC composites manufactured using a spark plasma sintering (SPS) method, a new sintering technique in development for poorly sinterable ceramic materials, was analysed by the scanning electron microscopy‐electron backscattered diffraction (SEM‐EBSD) method. Their crystallographic features have been compared with those of a conventionally sintered specimen using a pressureless sintering (PLS) method. In the composite sintered by PLS, (0001) planes of ZrB₂ were orientated in the direction parallel to the specimen surface (RD) but (101 0) and (211 0) planes randomly orientated. In the case of SPS, (0001) planes of ZrB₂ were orientated normal to the specimen surface (ND) and weakly to the RD. In both cases of PLS and SPS, ZrC grains had a randomly orientated grain structure. The distribution of grain boundary misorientation of PLS and SPS‐processed composites showed the same tendency that high‐angle boundaries were more prevalent than low‐angle boundaries. But in the case of ZrC grains in the SPS sample, the proportion of CSL boundaries with low sigma value (3, 5, 7, 9, 11) was relatively larger.     

The integration of experimental in-situ EBSD observations and numerical simulations: a novel technique of microstructural process analysis

The combination of subgrain‐ and grain‐scale microstructural data collected during in‐situ heating experiments and numerical simulations of equivalent microstructural development offers an innovative and powerful tool in the advancement of the understanding of microstructural processes. We present a system that fully integrates subgrain‐ to grain‐scale crystallographic data obtained during in‐situ observations during heating experiments in a scanning electron microscope and the two‐dimensional hybrid numerical modelling system Elle. Such a system offers the unique opportunity to test and verify theories for microstructural development, as predictions made by numerical simulations can be directly coupled to appropriate physical experiments and, conversely, theoretical explanations of experimental observations should be testable with numerical simulations. Discrepancies between data obtained with both techniques suggest the need for an in‐depth investigation and thus open up new avenues of theory development, modification and verification. In addition, because in numerical models it is possible to select the processes modelled, the effect of individual processes on the microstructural development of a specific material can be quantified. To illustrate the potential and methodology of the so‐called EBSD2Elle system, two in‐situ experiments and their equivalent numerical experiments are presented. These are static heating experiments of (a) an annealed Ni‐foil coupled with a front tracking model for grain growth and (b) a cold deformed rock salt with kinetic Monte Carlo simulations for subgrain growth.     

EBSD investigation of the microstructure and texture characteristics of hot deformed duplex stainless steel

The microstructure and crystallographic texture characteristics were studied in a 22Cr‐6Ni‐3Mo duplex stainless steel subjected to plastic deformation in torsion at a temperature of 1000 °C using a strain rate of 1 s^?1. High‐resolution EBSD was successfully used for precise phase and substructural characterization of this steel. The austenite/ferrite ratio and phase morphology as well as the crystallographic texture, subgrain size, misorientation angles and misorientation gradients corresponding to each phase were determined over large sample areas. The deformation mechanisms in each phase and the interrelationship between the two are discussed.     

Electron backscatter diffraction applied to lithium sheets prepared by broad ion beam milling

Due to its very low hardness and atomic number, pure lithium cannot be prepared by conventional methods prior to scanning electron microscopy analysis. Here, we report on the characterization of pure lithium metallic sheets used as base electrodes in the lithium‐ion battery technology using electron backscatter diffraction (EBSD) and X‐ray microanalysis using energy dispersive spectroscopy (EDS) after the sheet surface was polished by broad argon ion milling (IM). No grinding and polishing were necessary to achieve the sufficiently damage free necessary for surface analysis. Based on EDS results the impurities could be characterized and EBSD revealed the microsctructure and microtexture of this material with accuracy. The beam damage and oxidation/hydration resulting from the intensive use of IM and the transfer of the sample into the microscope chamber was estimated to be <50 nm. Despite the fact that the IM process generates an increase of temperature at the specimen surface, it was assumed that the milling parameters were sufficient to minimize the heating effect on the surface temperature. However, a cryo‐stage should be used if available during milling to guaranty a heating artefact free surface after the milling process. Microsc. Res. Tech., 78:30?39, 2015. © 2014 Wiley Periodicals, Inc.     

Development of high‐temperature strain instrumentation for in situ SEM evaluation of ductility dip cracking

Nowadays, the implementation of sophisticated in situ electron microscopy tests is providing new insights in several areas. In this work, an in situ high‐temperature strain test into a scanning electron microscope was developed. This setup was used to study the grain boundary sliding mechanism and its effect on the ductility dip cracking. This methodology was applied to study the mechanical behaviour of Ni‐base filler metal alloys ERNiCrFe‐7 and ERNiCr‐3, which were evaluated between 700°C and 1000°C. The ductility dip cracking susceptibility (threshold strain; ε_min) for both alloys was quantified. The ε_min of ERNiCrFe‐7 and ERNiCr‐3 alloys were 7.5% and 16.5%, respectively, confirming a better resistance of ERNiCr‐3 to ductility dip cracking. Furthermore, two separate components of grain boundary sliding, pure sliding (S_p) and deformation sliding (S_d), were identified and quantified. A direct and quantitative link between grain boundary tortuosity, grain boundary sliding and ductility dip cracking resistance has been established for the ERNiCrFe‐7 and ERNiCr‐3 alloys.     

Non‐Contact Evaluation of Osmosis‐Induced Shrinkage and Swelling Behavior of Articular Cartilage In‐Situ Using High‐Frequency Ultrasound

Abstract

The aim of the present study was to use high‐frequency ultrasound for the investigation of the transient osmosis‐induced free shrinkage‐swelling behaviors of normal articular cartilage in situ. Full‐thickness cartilage‐bone specimens were prepared from normal bovine patellae. The transient shrinkage and swelling strains of the cartilage induced by changing the bathing solution between physiological saline (0.15 M) and hypertonic saline (2 M) were monitored using a 50 MHz focused ultrasound beam. Both shrinkage and swelling strains showed temporary overshoots, followed by relaxation phases. The absolute peak value of the shrinkage strain (1.01%±0.62%) was significantly larger (p<0.05) than that of the swelling strain (0.40%±0.33%). It was found that the change of the mean ultrasound speed in cartilage could be approximately represented by an exponential function of time after the change of saline concentration.

This study successfully demonstrated that a high‐frequency focused ultrasound beam could be used to monitor the transient osmosis‐induced deformation of articular cartilage in a non‐contact way. Since the osmosis‐swelling behavior of cartilage relates to its compositional and structural characteristics and degeneration status, the reported ultrasound method may have potential for the characterization of cartilage degeneration, such as osteoarthritis.     

High resolution surface morphology measurements using EBSD cross-correlation techniques and AFM

The surface morphology surrounding wedge indentations in (0 0 1) Si has been measured using electron backscattered diffraction (EBSD) and atomic force microscopy (AFM). EBSD measurement of the lattice displacement field relative to a strain-free reference location allowed the surface uplift to be measured by summation of lattice rotations about the indentation axis. AFM was used in intermittent contact mode to determine surface morphology. The height profiles across the indentations for the two techniques agreed within 1 nm. Elastic uplift theory is used to model the data.     

Characterization of the three-dimensional structure of a metallic foam during compressive deformation

X‐ray microtomography has been employed to collect three‐dimensional images of aluminium closed‐cell foam, enabling the internal structure to be characterized in three dimensions. An experimental technique and image analysis approach has been developed, and is described, in terms of the labelling of cells and the extraction of quantitative data such as the cell volume and cell compression. An in situ compressive deformation experiment has been performed on a single sample in order to illustrate the approach. The effect of the three‐dimensional cellular structure on the mechanisms of deformation suggests not only the position of large cell volumes to be very important in the local concentration of stress, but also the distribution of cell volumes of immediate neighbours.     

Experimental simulation of phosphites additives tribochemical reactions by gas phase lubrication

Abstract

Tribochemical reactions of phosphites additives on steel surface have been simulated by gas phase lubrication. Trimethylphosphite (TMPi), P(OCH₃)₃, has been used as model molecule for phosphites additives. It has been introduced under gas phase up to 5 hPa in a new tribometer dedicated to gas phase lubrication. Friction tests have been carried out at ambient temperature and 100°C. Chemical analyses by X-ray photoelectron spectroscopy and by Auger electron spectroscopy have been conducted inside and outside of the track. Two kinds of analysis have been carried out: ex situ and in situ surface analyses after tribological test. Indeed, a new environmentally controlled tribometer allows friction test then accurate analyses without air exposure of the formed tribofilm. Tribotests conducted under TMPi gas phase show a reduction of friction coefficient until 0˙2 instead of 1˙4 under high vacuum. Jointly, formation of tribofilm has been confirmed by optical microscopy and ex situ chemical analysis. Comparison between analyses performed inside and outside of the wear scar indicates that the friction induces the formation of phosphide compound that could reduce friction. Moreover analyses show the formation of methoxy group (CH₃O) and carbonate originally from the decomposition of TMPi under friction into H₂ and CO. In situ analyses clearly show the importance to investigate an uncontaminated tribofilm in order to obtain a better characterisation of it and then a better comprehension of the tribochemical mechanisms.