The use of charging effects in Al/Al2O3 metal matrix composite materials as contrast mechanism in the SEM

Abstract

In Al/Al2O3 MMC's the metal/ceramic interfacial structure is of great concern because aluminum does not wet (i.e. bond) well to alumina. One proposed method to overcome this problem is to form a magnesium-rich spinel (MgAl2O4) as an additional phase between the aluminum matrix and the alumina particle. The spinel forms by diffusion of Mg from the matrix and improves the bonding. Typically the SEM would be the most suitable instrument to study the spinel, but this particular material combination (alumina/spinel) does not have sufficient secondary or backscattered electron contrast to allow for normal imaging. The purpose of this work was to develop a technique for examining the growth and morphology of this spinel at the Al/Al2O3 interface. Samples of an Al/Al2O3 MMC with a spinel at the particle interface were prepared according to standard metallographic procedures. Certain samples were sputter coated with a gold film of approximately 12 nm thickness; other samples were examined uncoated. Nonconductive, uncoated specimens charge under the incident electron beam if the accelerating voltage is below E1 or above E2 in Figure 1. In both of cases (below E1 and above E2) the number of electrons entering the sample is higher than the number of electrons leaving the sample. The resolving power of the SEM is usually degraded by this effect and therefore nonconductive specimens are coated with a layer of conductive material prior to observation. Figure 2 shows how this effect can create contrast between two materials due to its effect on the secondary electron detector bias voltage. Figure 3 shows that this contrast mechanism exists for the material combination alumina/spinel. The secondary electron image of a coated sample (3a) shows almost no contrast between alumina and spinel whereas the uncoated sample (3b) shows good contrast due to the different charging characteristics of the materials. The alumina charges stronger than the spinel and appears brighter in the image. The assumption that the effect is due to secondary electrons is supported by Figure 4. The micrograph in Figure 4a was obtained by backscattered electrons only and shows poor contrast whereas the micrograph in Figure 4b was obtained by secondary and backscattered electrons and shows good contrast. Figure 5 shows micrographs obtained at different operating voltages. The reduction in contrast at lower operating voltages is due to reduced charging.