A shock recovery experiment for mixing nickel and boron powder was performed by a flyer plate impact technique. The flyer velocity was in the range of 0.7–1.4 km s −1, and the shock pressure was calculated to be 4–11 GPa by the impedance matching method. The shock-treated sample was characterized by X-ray diffraction analysis, optical microscopy and transmission electron microscopy. The shock wave induces a reaction between the nickel and boron powder particle. The amount of the shock-synthesized intermetallic compounds is increased with increasing shock pressure. At a shock pressure of 11 GPa, a bubble-like structure is formed by the interaction between the powder particles. Transmission electron microscopy analysis reveals the presence of nano-scale nickel particles in the recovered samples. The shock compression proved useful for the formation of unique microstructures.