Issue 30

G. Bolzon et alii, Frattura ed Integrità Strutturale, 30 (2014) 31-39; DOI: 10.3221/IGF-ESIS.30.05 32 Factors governing the scale growth process may influence the mechanical properties and the adhesion to the steel substrate of the corrosion layer [5, 6] and the possibility of ensuring further adequate protection. These characteristics can be verified by means of indentation tests, which allow identifying the failure modes and calibrating the mechanical properties of materials. The maximum force applied by commonly available instrumentation can vary in a wide range (from mN to kN) and tests can be performed at different penetration depths. The geometry of the indenter tip can also be appropriately selected. In particular, rounded conical (Rockwell [7]) and sharp pyramidal (Vickers [8]) tips can be used to obtain complementary information. The material characteristics are reflected by the indentation curves, which correlate the displacement of the indenter tip to the exerted force. This information can be exploited to recover the microscopic or macroscopic mechanical properties of materials either in laboratory [9] or directly on components, possibly in situ [10]. Specific application of indentation techniques complemented by inverse analysis tools have been recently considered for the diagnostic analysis of pipeline systems [11], with the ultimate aim to prevent failures associated to progressive degradation phenomena, which may be assisted by the environmental conditions [12]. Methodologies suitable to identify the characteristics of coatings [13] and interfaces [14] in layered systems have been developed. Indentation curves can also reveal spall or cracking attitude depending on the ductility or the brittleness of the components [15]. The main results of an indentation study performed on the corrosion products grown on pipe steel samples are summarized in this contribution. Figure 1 : Morphology of carbonate scales obtained at 1 bar (a) [17] and 170 bar (b) CO 2 pressure: SEM micrographs with SE (Secondary Electrons) at the same magnification (Marker: 50 µm). M ATERIALS AND METHODS 65 pipeline steel [3] and J55 casing steel [16] were considered. The materials have different composition and different but comparable mechanical properties, listed in Tab. 1 and Tab. 2. Iron carbonate (FeCO 3 ) films were grown on polished and degreased square samples (20 × 20 mm 2 , 3 mm thickness) inserted in Hastelloy C276 autoclave in saturated CO 2 conditions at 70°C. The substrate was exposed for 68 hours to a synthetic fluid, with composition reported in Tab. 3. Specimens were observed with optical and electronic microscope. X ray diffraction (XRD) analysis was performed to identify scale composition. Details on specimen preparation and characterization are reported in [17] and [18]. C Si Mn P S Cr Ni Mo Cu Nb Ti Al V N X65 0.048 0.21 1.40 0.0220 0.002 0.018 - 0.200 0.01 0.4 0.007 0.04 - - J55 0.350 0.39 0.87 0.0015 0.008 0.130 0.12 0.018 0.23 - - 0.007 <0.01 - Table 1 : Chemical composition of the steel substrates (max %). The mechanical response of the specimens was investigated by indentation tests, performed with rounded (Rockwell [7]) and sharp (Vickers [8]) tips at 100 N and 200 N maximum load in a Zwick/Roell ZHU 0,2 equipment. The different characteristics of the surface layers were clearly reflected by the indentation curves, shown in Fig. 4 and Fig. 5 for X65 steel substrate. X