A kind of novel absorption material Nd4YFe88.5B6.5 was prepared by vacuum smelting, different ball milling time and proper annealing. The properties of the samples were tested. Results show that the microwave absorption values of all the unannealed and annealed samples are high and have a narrow range fluctuation. They increase with ball milling time prolonging and are improved greatly after annealing. The sample milled for 40 h owns the max absorption of 55.287 dB at the frequency of 10.63 GHz, while its absorption is improved greatly after annealing for 15 min at 550 oC, and the max absorption reaches to 132.415 dB at the frequency of 12.43 GHz. The causes of higher absorption properties were also discussed.