An attempt was made in the present work to study the compressive strength and microstructure of geopolymer containing high calcium fly ash (HCFA) and silica fume. Concentration of sodium hydroxide solution 8M, 10M, 12M & 14M, liquid to binder ratio 0.5 and sodium hydroxide to sodium silicate ratio 2.5 were selected for the mixes. Geopolymer mortar test results indicated that the mix with 40% silica fume by the weight of HCFA yielded higher compressive strength under ambient curing. The XRD pattern typically shows the major portion of amorphous phase of geopolymer. The existence of C-A-S-H gel, N-A-S-H gel and hydroxysodalite gel products were observed through SEM which developed dense microstructure and thus enhanced strength of HCFA and silica fume geopolymer.