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In order to realize the photocatalysis of TiO2 in the sunlight and directly apply it to waste water treatment, the Gd-doped TiO2 nanofibre was synthesized using two-step synthesis method as follows: Firstly, potassium carbonate, titanium dioxide and proper gadolinium oxide (dopant) were calcined in the muffle at high temperature and the doped gadolinium K2Ti4O9 fibres were obtained; secondly, the fibre was heated using glycerol as solvent until Gd-doped TiO2 nanofibres were obtained. The synthesized samples were characterized using scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The results show that Gd-doped TiO2 nanofibre heat-treated by glycerol solvent can inhibit the agglomeration, so the grain diameter of the fibre is smaller than that without heat-treated with glycerol. Meanwhile, the diameter of the fibre decreases with the increase of the heating temperature and time. 97%- 98% of Gd-doped TiO2 nanofibre is anatase. The photocatalysis results showed that the photocatalysis activity of Gd-doped TiO2 nanofibre is just a little lower than that of TiO2 powder.