Radiotherapy is a novel, non-invasive cancer treatment. Radioactive hollow microspheres, i.e., microcapsules, are attractive for in situ cancer radiotherapy because they can effectively reach tumors without settling in blood vessels. In particular, microcapsules 20-30 (im in size are expected to exhibit not only a radiotherapy effect but also embolization that blocks the nutrient supply to cancer cells. p-ray irradiation is the most suitable source for in situ radiotherapy because of its moderate range. Several kinds of p-emitting yttria (Y2O3) microcapsules have therefore been developed. Yttrium phosphate (YPO4) should have a longer irradiation effect than that of Y2O3 because the half-life of 31P (14.3 days) is longer than that of 90Y (64.1 hours). However, the preparation of YPO4 microcapsules has not been reported to date. In the present study, YPO4 microcapsules were fabricated using a water/oil (W/O) emulsion prepared by first dispersing a YPO4 sol into toluene containing a surfactant, with mechanical homogenization. The emulsion was then added into butanol to dehydrate the water phase and precipitate microcapsules. These were then heat-treated to improve their mechanical strength and chemical stability. Microcapsule fragility at low YPO4 sol concentrations in the water phase was attributed to the thinness of the microcapsule shell. The size of the microcapsules decreased with increasing emulsification speed. The chemical stability of the prepared microcapsules is similar to those of previously reported YPO4 and Y2O3 microspheres in weakly acidic conditions. Thus, little leakage of radioactive species into nearby healthy tissues is expected. The obtained microcapsules are expected to be highly effective for cancer radiotherapy.