The synthesis and characterization of nanosized zinc oxide and its nanofluid in a polyvinyl alcohol (PVA) matrix have been done in the present investigation. Crystalline zinc oxide nanoparticles are synthesized using single-step chemical method while the nanofluids are prepared by the dispersion of nanoparticles in PVA solution using an ultrasonicator. The prepared nanoparticles are characterized using X-ray diffraction, SEM–EDX and UV–visible spectrum. The particle size distribution measurement is carried out by acoustic particle sizer. The ultrasonic velocities are measured in the synthesized nanofluid under different physical conditions using an ultrasonic interferometer. It is found that the degree of crystallinity of nanoparticles depends on the evaporation rate during its synthesis and ultrasonic velocity has non-linear relation with temperature for the present nanofluid.