The solid solution of trirutile-type MSb
2O
6 (M=Cu, Zn, Mg, Co and Ni) and TiO
2 with the molar rates x=0.125, 0.25, 0.5 and 0.75 in (MSb
2O
6)
x(TiO
2)
1-x was prepared by a solid state reaction. The results showed that the solid solutions were formed except for (MSb
2O
6)
0.75(TiO
2)
0.25 (M=Mg and Co) and x=0.50 and 0.75 in (NiSb
2O
6)
x(TiO
2)
1-x, and were crystallized in trirutile type structure. Diffuse reflectance spectroscopy measurement for their powders indicated that the energy bandgaps were approximately 2.1 eV for (CoSb
2O
6)
x(TiO
2)
1-x (x=0.125, 0.25 and 0.5), and were approximately 2.6 and 2.4 eV for (NiSb
2O
6)
x(TiO
2)
1-x (x=0.125 and 0.25) and (CuSb
2O
6)
x(TiO
2)
1-x (x=0.125, 0.25, 0.5 and 0.75), respectively. The photocatalytic activity for visible light was observed in (CoSb
2O
6)
x(TiO
2)
1-x and (CuSb
2O
6)
x(TiO
2)
1-x.
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