Single crystals of Li3BP2O8 were prepared by heating a mixture of starting materials with a Li : B : P molar ratio of 22 : 11 : 13 at 933 K in air and by cooling at a rate of -10 K h-1. The X-ray diffraction (XRD) reflections of a single crystal were indexed with triclinic cell parameters: a = 5.1888(5) Å, b = 7.4118(7) Å, c = 7.6735(7) Å, α = 101.18(1)°, β = 105.07(1)°, γ = 90.34(1)° (space group P1̄ (no. 2)). In the crystal structure of Li3BP2O8, BO4 and PO4 tetrahedra share O atoms and form one-dimensional 1∞[BP2O 8]3- chains along the c-axis direction. A polycrystalline Li3BP2O8 bulk sample was synthesized by the solid state reaction of Li4P2O7 and LiPO 3 prepared from the starting materials in advance with H 3BO3 at 923 K. The lithium ion conductivities measured for the polycrystalline sample by the AC impedance and DC methods were 1.5 × 10-5 S cm-1 at 583 K and 6.0 × 10-8 S cm-1 at 423 K, respectively.
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