Sonochemical treatment were employed to produce catalysts containing mixtures of nickel oxide and cerium oxide supported by alumina with different ratio, 1:1, 1:2 and 2:1 and each ratio was sonicating for 15, 45 and 75 minutes. The catalysts were characterized by X-ray diffraction (XRD), BET surface area measurement, scanning electron microscope (SEM) with energy dispersive X-ray analysis (EDX), transmission electron microscope (TEM) and temperature-programmed reduction (TPR) in H2. The syngas production was detected using temperature programmed gasification (TPG) and it was done under 5% oxygen in helium. The coconut shell in powder form (3 μm) was used as a feedstock. The results found that XRD patterns showed all studied catalyst were matching to the XRD patterns standard of NiO, CeO2 and alumina, indicating that the catalysts produced through this method consist of the mentioned compound. EDX results further confirmed that all of the elements contain inside the synthesized catalyst were Ni, Ce, O, Al. 1:145min showed the highest syngas production (H2/CO) with ratio 0.76 due to the smaller particle size and higher surface area which increase the contact frequency between the catalyst and coconut shell. The catalyst produce the highest syngas production (H2/CO) with ratio 0.76 which is near to the optimum ratio,1.