The crystal and defect structures of coarse-grained crystals of La(2/3-x)Li(3x)TiO3 grown from the melt by the Tammann-Stöber method were studied by transmission electron microscopy and powder X-ray diffraction. The as-grown crystals of La(2/3-x)Li(3x)TiO3 have a Li-poor composition of La(0.57)Li(0.29)TiO3 and a diagonal-type unit cell of 2(1/2)a(p) x 2(1/2)a(p) x 2a(p) with the tetragonal symmetry [space group: P4/nbm (#125)] due to both the La-cation ordering and the tilting of TiO6 octahedra. The secondary La2Ti2O7 phase precipitates in the form of plates in the La(2/3-x)Li(3x)TiO3 phase with the orientation relationships of 001(p)//[100](La2Ti2O7) and {110}(p)//(001)(La2Ti2O7), which may cause detrimental effects to ionic conductivity.
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