A simple and economical device to process Ti cylinders with elongated porosity by freeze-casting techniques: Design and manufacturing

Nowadays, the development of materials with gradient porosity is an important aim for many applications, especially in the field of bone tissue replacement. This research work shows the design and manufacture of a simple and economical device to process Ti cylinders with elongated and high interconnected porosity by freeze-casting techniques. The influence of the vessel material on the internal lamellar structure of the porous Ti samples is also studied. The device has been validated with: (i) a thermal gradient from -10 °C at the cold surface to 20 °C at the hot surface; and (ii) a cylindrical vessel with 12 mm diameter of alumina or Teflon. These working conditions have allowed maintaining the freezing conditions during the full process (alumina vessel: 30 minutes; Teflon vessel: 3 hours). After the solidification of the Ti aqueous suspension, the ice is sublimated (24 hours at -50 °C and 0.070 mbar). Then, the resulting powder is sintered (1150 °C for 5 h at high vacuum ~ 10^-5 mbar), obtaining the porous Ti sample with the final structural strength. Finally, a detailed study of the most relevant porosity features is performed: porosity ratio and interconnectivity degree by Archimedes' method, and size and shape of the pores by image analysis at three different zones along the longitudinal cross section. The results indicate the viability of the device to enhance the directional freezing and thus, the elongated porosity. Teflon vessel present the best results, with an average porosity ratio and porosity size of 39.5 % and 123.3 µm, respectively. This suggests an optimal biomechanical and bifunctional balance of this porous material.