A new method for in-situ studies of nucleation in bulk metals based on high energy synchrotron radiation is presented. Copper samples cold rolled 20% are investigated. The crystallographic orientations near triple junctions are characterized using non-destructive 3DXRD microscopy before, during, and after annealing for 1 hour at 290°C. This method allows in-situ identification of new nuclei and the deformed material, which spawns the nuclei. Also, since data is acquired during annealing nucleation kinetics can be studied.