For decades, superfluid helium has attracted the interest of the scientific community as an extremely pure realisation of a quantum liquid, only accessible at temperatures close to absolute zero. Previously, helium films have only been observed directly using X-rays. However, this method is limited to temperatures above 1 K due to the high levels of energy deposition, and it also suffers from an inability to distinguish between helium isotopes. Here we show that a 3He layer on top of a phase separated mixture film at 170 mK gradually dissolves into the 4He with increasing temperature. We also observe an anomaly in film behaviour near 300 mK and unexpected restoration of the layered structure at 1.5 K which is consistent with a re-entrant phase transition leading to the suppression of superfluidity in the film near 300 mK. Our successful application of neutron scattering to study helium films at ultra-low temperatures opens up new possibilities for future research.