An investigation into the properties of nanocrystalline(NC) materials with sample lengths less than 30 mm seems to be a challenge by using conventional mechanical spectroscopy(MS).We use a newly developed frequency modulation acoustic attenuation mechanical spectroscopy(FMAA-MS) to investigate phase transition in Ni68Fe32 NC alloy(22nm) where the length of the sample is 10mm.An inteal friction peak accompanied by an abrupt increase in resonant frequency occurs at 641 K, which originates from order-disorder phase transition, confirmed by a vibrating sample magnetometer and differential scanning calorimetry.