The use of combined three-dimensional electron backscatter diffraction and energy dispersive X-ray analysis to assess the characteristics of the gamma/gamma-prime microstructure in alloy 720Li.

Multiple three-dimensional reconstructions of a γ/γ' phase structure in Alloy 720Li have been carried out by employing a serial milling technique with simultaneous electron backscatter diffraction (EBSD) and energy dispersive x-ray (EDX) analysis data collection. Combining EBSD data with EDX is critical in obtaining maps to distinguish between the chemically differing, but crystallographically similar γ and γ' phases present in the alloy studied. EDX is shown to allow the differentiation of γ and γ' phases, with EBSD providing increased grain shape accuracy. The combination of data sources also allowed identification of coherent γ/γ' phase interfaces that would not be identified using solely EBSD or EDX. The study identifies a region of grain banding within the alloy, which provides the basis for a three-dimensional comparison and discussion of γ' phase size between coarse and fine grain regions, whilst also identifying coherent γ' phase interfaces, possible only using both EDX and EBSD systems simultaneously. The majority of the γ' phase lies in the range of 1-10 µm in non-banded regions, with a detectable particle size limit of 500 nm being established. The validity of the reconstruction has been demonstrated using an electron interaction volumes model, and an assessment of the validity of EBSD and EDX data sources is discussed showing γ' phase connectivity in all dimensions.

Combined EBSD/EDS tomography in a dual-beam FIB/FEG-SEM.

An automated method for collecting combined three-dimensional (3D) electron backscatter diffraction (EBSD)/energy dispersive spectroscopy (EDS) data sets on a dual-beam focused ion beam (FIB)/field emission gun scanning electron microscope (FEG-SEM) microscope is described. The method uses simple scripting files on the dual beam to move between the EBSD collection and the FIB slicing positions, which are linked to a commercial EBSD data collection programme. The EDS data are collected simultaneously with the EBSD patterns analogous to combined two-dimensional (2D) EBSD/EDS. The technique has been successfully applied to study both the interdiffusion zone between a coating and a substrate and a complex multi-phase coating on a nickel-based superalloy sample. This analysis is shown to enable the complex grain shapes, location of precipitates and phase interconnectivity within these samples to be determined without the ambiguities associated with 2D stereographic analysis.

Focused ion beam milling and ultramicrotomy of mineralised ivory dentine for analytical transmission electron microscopy.

The use of focused ion beam (FIB) milling for preparation of sections of mineralised ivory dentine for transmission electron microscopy (TEM) is investigated. Ivory dentine is essentially composed of fibrillar type-I collagen and apatite crystals. The aim of this project is to gain a clearer understanding of the relationship between the organic and inorganic components of ivory dentine using analytical TEM, in order to utilise these analytical techniques in the context of common skeletal diseases such as osteoporosis and arthritis. TEM sections were prepared in both single and dual beam FIB instruments, using two standard lift-out techniques, in situ and ex situ. The FIB sections were systematically compared with sections prepared by ultramicrotomy, the traditional preparation route in biological systems, in terms of structural and chemical differences. A clear advantage of FIB milling over ultramicrotomy is that dehydration, embedding and section flotation can be eliminated, so that partial mineral loss due to dissolution is avoided. The characteristic banding of collagen fibrils was clearly seen in FIB milled sections without the need for any chemical staining, as is commonly employed in ultramicrotomy. The FIB milling technique was able to produce high-quality TEM sections of ivory dentine, which are suitable for further investigation using electron energy-loss spectroscopy (EELS) and energy-filtering TEM (EFTEM) to probe the collagen/apatite interface.

Phase determination and microstructure of oxide scales formed on steel at high temperature.

Even in simple low-alloy steels the oxide scales that form during hot working processes are often a complex mixture of three iron oxide phases: haematite, magnetite and wustite. The mechanical properties, and hence descalability, are intimately linked with phase distribution and microstructure, which in turn are sensitive to both steel composition and oxidation conditions. In this study electron backscatter diffraction in the SEM has been used to characterize the microstructures of oxide scales formed on two compositions of low-alloy steel. The technique can unambiguously differentiate between the candidate phases to provide the phase distribution within the scale. This is used to investigate grain orientation relationships both within and between phase layers. It has been found that the strength of the orientational relationship between the magnetite and wustite layers is dependent on steel composition, and in particular Si content. In a low-Si (0.01 wt%) alloy only a very weak relationship was found to exist for a range of oxidation temperatures (800-1000 degrees C), whereas for the higher Si (0.37 wt%) alloy a strong relationship was observed under the same oxidation conditions. These orientational relationships are particularly important because, in this temperature range, the majority of oxide scale growth occurs at the magnetite/wustite interphase boundary.