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With BaCO3, MnCO3 and Yb2O3 as raw materials, the two new compounds, 12R-Ba4YbMn3O11.5 and 10H-Ba5YbMn4O14.5, were synthesized using traditional solid-state reaction at 1300°C. The chemical formulas of the composites were determined through EDS analysis and redox titration, the crystalline structure of the compounds were determined through selected area electron diffraction and Rietveld refinement based on powder X-ray diffraction. It was shown that the 12R-Ba4YbMn3O11.5 belonged to the R-3m space group with the lattice parameter of a =0.578 nm and c=2.850 nm; and the 10H-Ba5YbMn4O14.5 belonged to the P63/mmc space group with the lattice parameter of a =0.575 nm and c =2.377 nm.
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