The synthesis of Ho 3 + -Yb 3 + codoped titanate nanotubes was carried out successfully via a hydrothermal treatment method from a precursor powder. These novel nanotubes treated at RT, 100°C and 280°C were studied with the aim of determining their structural and optical properties. As the thermal treatment was increased, their upconversion emission becomes stronger. This behavior was related to reduction of hydroxyl groups and the water on the surface, which resulted in changes in the interlayer distances of the nanotubes.