A high-energy-ball-milling process was applied to the synthesis of the Rb
4Cu
16I
7Cl
13 crystalline phase, which was known to show high Cu
+ ion conductivity 3.4×10
1Sm
-1 at room temperature. CuCI, Cul, and RbCl were used as raw materials for the mechanical synthesis of the Rb
4Cu
16I
7Cl
13 phase. The ball mill treatment of the mixture of the raw materials more than l0h led to the formation of the Rb
4Cu
16I
7Cl
13 crystalline phase. The obtained Rb
4Cu
16I
7Cl
13 crystals showed high ion conductivity more than 10
1 Sm
-1 at room temperature, and the conductivity increased with an increase in milling time and reached a constant value of 1.8 x 10
1 Sm
-1 at 298 K for the sample ball-milled more than 20 h. The electronic polarization measurements with Wagner's methods suggested that main carrier of the electronic conduction of the ball-milled sample was positive hale and that the hale conductivity was 1.2×10
-11 Sm
-1 at 273 K. These measurements indicated that the Cu
+ ion transport number of the sample was almost unity.
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