SmOHCO3micro/nanoparticleswerepreparedinwater/oil(W/O)reversemicroemulsioncomposedofcetyltrimethylammoniumbromide(CTAB),n-octane,n-butanol,Sm(NO3)3·6H2Oandureaaqueoussolutionbythecouplingrouteofhomogeneousprecipitationwithmicroemulsion.ThenanoparticleswerecharacterizedandanalyzedbyX-raypowderdiffraction(XRD),thermalgravimetricanddifferentialthermalgravimetricanalysis(TG-DTG),Fouriertransforminfraredabsorptionspectra(FT-IR)andscanningelectronmicroscope(SEM).TheresultsshowedthatthephaseSmOHCO3micro/nanoparticleswasinagreementwithpureorthorhombicphase.ThedifferentmorphologiesofSmOHCO3micro/nanoparticleswithgoodmonodispersityandsizewereobtainedbyregulatingthereactiontemperatureandreactiontime.PossibleformationmechanismsofthemorphologicalstructureofSmOHCO3wereproposedanddiscussed.