A laboratory preparation process of glass ceramics from nickel slag was introduced. The controlled heat treatment processes were carried out on the basis of differential scanning calorimetric (DSC) measurements. Mineral phase and microstructure of crystallized glass were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The modified Kissinger equation was employed to investigate the crystallization kinetic parameters, activation energy E and the k(Tp). The Avrami exponent, n, was calculated by Augis-Bennett equation. Analysis indicated that the glass with 10%TiO2 added was peril to crystallize, of a large value of k(Tp), its k(Tp) is 0.244, E is 522.76kJ/mol and n is 3.42. The crystal phase is diopside.