Ultra-black materials with low reflectivity can be applied in many fields of science and technology. We deposited nickel-phosphorus alloys (Ni-P) on copper substrate with the electroless plating method and etched the electroless plating with nitric acid in order to build ultra-black surface. On the one hand, the components of the Ni-P ultra-black surface layer were investigated by XRF and XPS. SEM represented that there are innumerable conical holes with the different diameters on the surface. XRD showed that the whole surface has become amorphous. On the other hand, compared to electroless blackening film by oxidation and black chromium plating materials, the Ni-P ultra-black surface showed lower wavelength dependence and lower reflectance in the range of 380–780 nm. In addition, the temperature of the sample with the Ni-P ultra-black surface increased more highly and quickly compared to the black chromium plating film after exposure in an IR laser for about half an hour.