Focused ion beam sample preparation of continuous fibre‐reinforced ceramic composite specimens for transmission electron microscopy

Abstract

The microanalysis of interfaces in fibre-reinforced composite materials is dependent on the successful preparation of specimens suitable for transmission electron microscope (TEM) inspection. Ideal samples should possess large amounts of structurally intact and uniform thin area in the fibre/matrix interface regions of the samples. Because fibre/matrix interfaces in this class of materials are often designed to fail under mechanical stress, conventionally prepared samples are prone to interfacial failure and differential thinning, both of which preclude detailed TEM microanalysis. These effects were seen in a conventionally dimpled and ion-beam-thinned specimen prepared from a continuous fibre reinforced ceramic composite composed of CaWO4-coated Nextel 610TM fibres in an alumina matrix. The dimpled specimen showed large amounts of interfacial failure, with only thick regions of the specimen left intact. To overcome these limitations, a focused ion beam (FIB) technique was applied to this same material. The superiority of the FIB-produced sample is evident in both the morphology and scanning transmission electron microscopy analyses of the sample.

Ultrathin section preparation of phyllosilicates by Focused Ion Beam milling for quantitative analysis by TEM-EDX

“…In other words, a thin section with a thickness of 200 nm is preserved to 80%. Similar results have been obtained by other authors for other materials, as Kim and Dravid (2000) for Al2O3 and CaWO4. With the FIB used in this study, it is possible to decrease the beam intensity (5000 to 30 pA) but not the beam current voltage under 30 kV without deteriorating the quality of the working image, which is now possible with the dual-beam FIB systems.…”

Tools for the Characterization of Biomass at the Nanometer Scale

“…Most published examples of FIB involve inorganic semiconductor materials (78, 79) or inorganic composites (80), but use with soft materials is also possible. Human hair and housefly eye (81) represent biological specimens.…”

Introduction to Focused Ion Beams

“…Several selected articles are referenced below; the reader is encouraged to perform their own up-to-date search as well as reviewing the following articles. Kim & Dravid (2000), discuss FIB preparation of continuous fiber reinforced ceramic composites for TEM analysis. Gianuzzi et al (1998) discuss applications of the FIB LiR-Out technique for TEM specimen preparation, illustrating the versatility of the technique with applications including galvanized steel and S i c fibres.…”