PtCo hard magnets have specialized applications owing to their relatively high coercivity combined with corrosion resistance and ductility. Increased intrinsic coercivity has been recently obtained by rapid solidification processing of PtCo alloys containing boron. After rapid solidification by double anvil splat quenching and subsequent annealing for 30 minutes at 650°C, an alloy with composition Pt42Co45B13 (at.%) exhibited intrinsic coercivity up to 14kOe. This represents a significant improvement compared to the average coercivities in conventional binary PtCo alloys of 5 to 8 kOe.Rapidly solidified specimens of Pt42Co45B13 (at.%) were annealed at 650°C and 800°C for 30 minutes. The magnetic behavior was characterized by measuring the coercive force (Hc). Samples for TEM analysis were mechanically thinned to 100 μm, dimpled to about 30 nm, and ion milled to electron transparency in a Gatan Duomill at 5 kV and 1 mA gun current. The incident ion beam angle was set at 15° and the samples were liquid nitrogen cooled during milling. These samples were analyzed with a Philips CM20T TEM/STEM operated at 200 kV.