In this work,CuFe2O4 hollow microspheres assembled with nanosheets(CuFe2O4 HMANs)were syn-thesized using a solvothermal method followed by an annealing treatment.The effects of annealing temperature on microstructure,chemical composition and gas sensing characteristics of as-prepared samples were investigated.The results showed that annealing treatment played a cru-cial role in the final products.All samples demonstrated hollow spherical morphology assembled with nanosheets or nanoparticles.The CuFe2O4 HMANs annealed at 400℃ exhibited the best n-type conductometric sensing properties toward low-concentration NH3 at 100℃ and 49% RH.The sensor response to 10×10-6 NH3 was 4.0 with a rapid response time of 32 s,and it even showed a response of 1.2 toward 1×10-6 NH3 at the same condi-tion,while a response of 3.95 to trimethylamine(TMA).The CuFe2O4 HMANs-based NH3 sensor also exhibited good selectivity and excellent reproducibility.Therefore,this work provided a novel promised sensing material of low-concentration NH3 and TMA for real-time monitoring.