New approach for FIB-preparation of atom probe specimens for aluminum alloys

Site-specific atom probe tomography (APT) from aluminum alloys has been limited by sample preparation issues. Indeed, Ga, which is conventionally used in focused-ion beam (FIB) preparations, has a high affinity for Al grain boundaries and causes their embrittlement. This leads to high concentrations of Ga at grain boundaries after specimen preparation, unreliable compositional analyses and low specimen yield. Here, to tackle this problem, we propose to use cryo-FIB for APT specimen preparation specifically from grain boundaries in a commercial Al-alloy. We demonstrate how this setup, easily implementable on conventional Ga-FIB instruments, is efficient to prevent Ga diffusion to grain boundaries. Specimens were prepared at room temperature and at cryogenic temperature (below approx. 90K) are compared, and we confirm that at room temperature, a compositional enrichment above 15 at.% of Ga is found at the grain boundary, whereas no enrichment could be detected for the cryo-prepared sample. We propose that this is due to the decrease of the diffusion rate of Ga at low temperature. The present results could have a high impact on the understanding of aluminum and Al-alloys.