The effect of two different milling devices, namely attrition mill versus vibration mill, on the reactivity of fly ash was studied. High calcium fly ash from 4th Thermal power station of Ulaanbaatar (Mongolia) was used for the experiments. The raw and processed samples were characterized by XRD, SEM, Particle size distribution, BET, Blaine surface area and density measurements. The efficiency of 1 hour milling was evaluated with the Blaine surface area set to be more than 5000 cm2/g. The physical and chemical properties of the attrition milled fly ash changed not much compared to the vibration milled samples. For example the d50 particle size became reduced from 29 μm to 6 μm by attrition milling and in vibration milled fly ash it was reduced to 7 μm. The density increased from 2.44 g/cm3 of raw fly ash to 2.84 g/cm3 and 2.79 g/cm3 in attrition and vibration milled samples, respectively. Mechanical milling revealed not only a particle size reduction but also the formation of a denser microstructure. As a result the vibration milled fly ash showed a weaker interaction with the alkaline solution (8 M NaOH used here) compared to the attrition milled fly ash. Consequently, compressive strength of the binder prepared using the attrition milled fly ash was higher, 61 MPa, while for vibration milled fly ash it was 49 MPa. For comparison unmilled fly ash, it was 21 MPa.