Abstract. This study was conducted in order to determine the effect of different particle size and pretreatment temperature to the crystallinity of leucaena leucocephala. The leucaena was pretreated by ionic liquid [1-ethyl-3 methylimidazolium acetate [Emim]Ac. There were three different particle sizes that have been tested in this experiment; less than 0.3 mm, 0.5 mm and 0.7 mm. In the other hand, the pretreatment temperature tested were 30℃, 60℃ and 90℃. The effect of particle size and pretreatment temperature to the crystallinity of leucaena was investigated by using X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The crystallinity index of the sample represents the percentage of crystalline materials. A lower in the cristallinity index indicated that the material has lower crystillinity, hence give more benefit to the cellulose hydrolysis. From XRD analysis, it shows that the cristallinity index of leucaena decreased with decreasing particle size and increasing pretreatment temperature. SEM analysis also shows that the structure of leucaena has more irregular, porous and destroyed structure with decreasing particle size and increasing pretreatment temperature. Thus, the result from this experiment shows that the smaller particle size and higher pretreatment temperature would provide a more accessible surface area to enhance the cellulose hydrolysis.