The iron doped compensation silicon materials were prepared by diffusing iron into p-type silicon of 4.8Ω•cm and n-type silicon of 10 Ω•cm using high temperature diffusion method. The resistivity of doped samples was measured at room temperature and photophobic condition. The samples were also analyzed using X-ray diffraction method. The effects of iron-doping on resistivity of different Si materials were studied. The results show that deep level impurity iron has greater influence on resistivity of p-type silicon than that of n-type silicon, the resitivity of iron-doped p-type silicon is much more than that of iron-doped n-type silicon, and the resistivity of the iron doped p-type silicon obtains the maximum value of 7 246 Ω•cm when the doping process is carried out at 1 200 ℃ for 1 h with the surface density of the iron dopant source being 1.74×10–5 mol/cm2.