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The structure of NdFeO3 doped Yb using solid state reaction method have been investigated. In this paper, Nd1-xYbxFeO3 samples were synthesized by varying the molar ratio of Yb at x=0.01, x=0.05 and x=0.10, respectively. All samples then characterized using X-ray diffractometer to obtain their crystal structure and phase. The Rietveld refinement method that can be used in Rietica software was used to analyse lattice parameters of the samples. Result of X-ray diffraction shows the presence of Yb did not affect the crystal structure of NdFeO3. The Rietveld refinement process shows that all samples have a good refinement indicating by the value of χ2 ranging from 1.2 to 1.4 and the good visualization of graph between experimental and calculation pattern. Further analyses of lattice parameters results will be explained in this paper.