Abstract: Ytterbium deuteride samples with atomic ratio of 2.90, 2.53 and 2.23 are produced by ytterbium reaction of deuterium at 400 ℃ and initial deuterium pressure of 6.53, 3.41 and 1.32 MPa, respectively. YbD 2.90 has a fcc sturcture and a 0=0.520 5 nm. A product of YbD 2.06 with orthorhombic ( a 0=0.587 0 nm, b 0=0.357 2 nm, c 0=0.679 4 nm) and another fcc sturcture ( a 0=0.523 3 nm) is produced by decomposing YbD 2.90 at 600 ℃. Both YbD 2.53 and YbD 2.23 are composed by fcc and orthorhombic structure. The results of thermo analysis indicate that there are three endothermic peaks on the DSC curves of four samples, and they represent the decomposed peak of fcc ( a 0=0.520 5 nm), fcc ( a 0= 0.523 3 nm ) and orthorhombic sturcture, respectively, and they will move to the low temperature side with the increase of D/Yb atomic ratio.