This study is for investigating the direct electro-deoxidation ofmixed TiO

2

-MnO

2

powder to prepare TiMn

2

alloy in molten calciumchloride. The influences of process parameters

such as sintering temperature

cell voltage

and electrolysis time

on the electrolysis processwere examined to investigate themechanismof alloy formation. The composition and morphology of the products were analyzed by XRD and SEM

respectively. The electrochemical property of TiMn

2

alloywas investigated by cyclic voltammetrymeasurements. The results showthat pure TiMn

2

can be prepared by direct electrochemical reduction of mixed TiO

2

/MnO

2

pellets at a voltage of 3.1 V in molten calcium chloride of 900 ℃ for 7 h. The electro-deoxidation proceeds from the reduction of manganese oxides to Mn

which is reduced by TiO

2

or CaTiO

3

to formTiMn

2

alloy. The cyclic voltammetrymeasurements using powder microelectrode show that the prepared TiMn

2

alloy has good electrochemical hydrogen storage property.