A modified blister test to study the adhesion of thin coatings based on local helium ion implantation

Abstract

A modified blister test has been developed based on helium ion implantation into selected areas of the metal substrate prior to the coating deposition. After a post-deposition thermal annealing, blisters are formed by agglomeration of the implanted gas at the ceramic–metal interface. This method can be used to control the pressure in the blister which eventually may lead to delamination at the periphery of the blister. A microsieve with a regular array of circular holes is used during the implantation to assure the initial blister size. Two different microsieves were employed in this work, with pore diameters of 1.5 and 4.5 μm, respectively. The distance between the centres of neighbour pores is twice the pore diameter. Scanning Electron Microscopy (SEM) and Confocal Scanning Optical Microscopy (CSOM) observations allowed the determination of the blistering parameters such as the radius, the height and the blister volume. From the gas content and these parameters, the work of adhesion or energy release rate can be obtained.

In this work, we present the first results of this blister test applied to W–C:H films and multilayers of Ti and Al deposited by Physical Vapour Deposition on polycrystalline copper substrates. The copper substrates were implanted with 34 keV He+ ions up to fluences of 3 and 5×1016 cm−2 before the deposition of the coatings and annealed afterwards in vacuum at temperatures from 773 to 1073 K for 30 min. Delamination of the Ti/Al multilayer coatings was already detected after annealing at 873 K with an energy release rate estimated to be 0.5 J m−2 at a typical helium pressure of 107 Pa. No delamination but only helium swelling was observed for W–C:H coatings annealed at 1073 K. Results of experiments on uncoated copper samples are also shown in order to explain the mechanism of helium bubble growth and helium release that causes the creation of the blisters.