Amorphous (a-LATP) powders with various nominal compositions of Li
1+xAl
xTi
2−x(PO
4)
3 (
x = 0, 0.3, 0.35, 0.4, 0.45, 0.5, 0.6) in the Li
2O-Al
2O
3-TiO
2-P
2O
5 (LATP) system, were prepared directly from a mixture of Li
2O, γ-Al
2O
3, anatase-type TiO
2, and P
2O
5 as the starting powder, using mechanical milling (MM) at room temperature. Crystalline LATP (c-LATP) powder with a NASICON-type structure was formed by the heat treatment of mechanochemically prepared a-LATP powder. In addition, heat-treated c-LATP (
x = 0.5, 0.6) powders included an impurity phase of crystalline Li
5AlO
4. The sintered c-LATP (
x = 0) pellet without Al
3+ doping exhibited a low electrical conductivity on the order of 10
−7 S cm
−1 at room temperature. On the other hand, the sintered Al
3+-doped c-LATP (
x = 0.3, 0.4, 0.45, and 0.5) pellets showed high electrical conductivities on the order of 10
−4 S cm
−1 at room temperature. The sintered c-LATP (
x = 0.45) pellet exhibited the highest lithium ion conductivity (2.9 × 10
−4 S m
−1) at 25°C and the lowest activation energy (30 kJ mol
−1).
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