The development of advanced materials, with complex microstructures, is a p
ermanent challenge to the development and application of new efficient tech
niques for microstructural characterization. In ceramic coatings on metals,
there exist a differential ion-milling ratio between both components, limi
ting in principle the use of conventional techniques. In this work, we repo
rt on a comparative study of TEM sample preparation techniques for plasma-s
prayed ceramic coatings. Firstly, we have used a procedure derived from the
conventional one (polishing, dimpling, ion milling), and alternatively a n
ew technique using focused ion-beam milling. The material selected for this
study is fine-grained alumina that was plasma-sprayed on a steel substrate
. The efficiency of both techniques is discussed along with the most signif
icant microstructural features of the material subject of study.