Single crystals of Li
4+xTi
5O
12 were prepared by means of electrochemical Li-ion intercalation technique using parent Li
4Ti
5O
12 single crystals. The obtained Li
4+xTi
5O
12(x=1.35)crystallizes in the cubic spinel-related type structre, space group
Fd3m, and lattice parameters of
a=8.346(3)Å and
V=581.3(5)Å
3. The Li-ion intercalated sites were successfully determined by single crystal X-ray diffraction. From the result, because of the structural restriction of the spinel structure, unfortunately, the theoretical capacity was revealed to be 175 mAh/g. New material Li
2Ti
6O
13 with rectangular tunnels was synthesized by Na
+/Li
+ ion-exchange method as one of the negative electrode material having a high capacity than Li
4Ti
5O
12. The Li
2Ti
6O
13 as determined the precise crystal structure by powder neutron diffraction and evaluated reversible Li insertion/extraction reaction.
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