A novel material, namely, Fe-containing lithium-metal triphosphate (LiM
2P
3O
10; M=Fe), has been synthesizedby wet-chemical method. The phase shows the monoclinic structure (
P2
1/
mC22h). The crystal chemistryand chemical structural characteristics have been analyzed by X-ray-diffraction (XRD), energy-dispersiveX-ray spectroscopy (EDS), and high-angle annular dark field scanning transmission electron microscopy(HAADF-STEM). Surface chemical composition, valence state, and chemical bonding and local structureanalysis have been performed by X-ray photoelectron (XPS) and Raman scattering (RS) spectroscopy. EDSand HAADF-STEM indicate the chemical homogeneity and purity of LiFe
2P
3O
10 samples. Both XPS and RSexperiments show the existence of an amorphous carbon deposit at the surface of the LiFe
2P
3O
10 particles.Comparison between XPS results for LiFePO
4 olivine and LiFe
2P
3O
10 revealed the change in the bindingenergy of Fe(II) ions. Studies of the local structure characterized by Raman scattering show the evolution ofthe chemical bonding with the increased number of interconnected PO
4 oxo-anionic groups. The electrochemicalcharacteristics of LiFe
2P
3O
10 demonstrate their applicability in lithium batteries.