Nano-FeNi alloy/ethanol sol and its nano-FeNi alloy have been successively prepared by pulsed laser ablation at the interface of flowing ethanol and rotative FeNi alloy target. The energy spectrum analysis shows that the weight ratio of constituents of the Fe and Ni in the nano-FeNi alloy particles is about 66 : 34. The shows that the nano-FeNi alloy particles’ original sizes are about 1–5 nm, and the particle sizes gradually become 10–50 nm due to self-congregation during 1–3 d. The XRD analysis indicates that the nano-FeNi alloy particles are almost in non-crystalline. It is found that there are one strong excitation peak at 311.00 nm and two weak excitation peaks at 273.00 and 347.00 nm, and there is one strong emission peak at 418.00 nm when it is excitated by 311.00 nm at room temperature from the fluorescence spectrum of nano-FeNi alloy/ethanol sol. The UV-Vis spectrum of nano-FeNi alloy/ethanol sol indicates that there exist one strong absorption peak which is splitted into 9 distinguished small peaks at about 230.00 nm and one weak exciton absorption peak at 275.00 nm. The FT-IR spectrum of nano-FeNi alloy/ethanol sol exhibits that the stretching vibration absorption peak of associating hydroxyl (v O?H) in the sol has the distinct blue shift, and confirms that the surface of nano-FeNi alloy particles has been modified by carbon-hydrogen organic group from ethanol decomposition in the producing process of the nano-FeNi alloy/ethanol sol
