31 Influence of Annealing in Vacuum on Dispersion Kinetics of Titanium. . .
489
Annealed samples were examined using scanning electron microscopes JCM6700 and JCM-5000 and an atomic force microscope Nanoscope III A with
micrograph recording. The Raman spectra of titanium and zirconium nanofilms
were obtained using a Renishaw inVia Raman microscope (Renishaw plc, Wottonunder-Edge, UK) at an excitation wavelength of 633 nm.
Using these micrographs, the area of substrate surface coated with metal film
islands was calculated by planimetric weighting method, i.e., by weighting of metalcoated sample parts images cut from micrographs [2]. The data obtained by this
method were analyzed as the dependence of sample surface area covered with metal
film fragments after annealing on annealing parameters (annealing temperature and
time).
31.3 Results and Discussion
Original titanium and zirconium films on both substrates were solid, without any
significant defects, and micrographs obtained using electronic scanning microscopes show only the uniform dark gray field.
During annealing of titanium film on the leucosapphire surface, at first, minor
signs of changes in the structure of the film appeared only as a result of its 2min heating up to 1300
◦ C. As a result of further exposition at this temperature for
5 min, film began to blister in part without losing its integrity, and the process rate is
slightly increased after a 10-min annealing (Fig. 31.1a), but the film still remained
solid. With increased exposition time up to 20 min at 1300
◦ C, the film is rapidly
disintegrated into large pieces. The similar pattern was observed with increase of
annealing temperature up to 1400
◦ C: the film is partially started to blister after
the 2-min exposition without losing its integrity; after a 5-min annealing, process
greatly intensified, and the film even started to crack (Fig. 31.1b). With further
exposition at this temperature for 10 min, quite long and wide cracks appear in the
film; and, finally, after a 20-min annealing, film completely disintegrated into large
fragments between which significant parts of free leucosapphire surface appear.
Annealing at 1500
◦ C has speeded up significantly the process of the titanium
film disintegration. Thus, after the 2-min annealing, film blistered intensively and
lost its integrity; after the 5-min exposition, it is cracked significantly; during
further exposition time increase of up to 10 min, film disintegrated into large
fragments (Fig. 31.1c); and after 2-min annealing at this temperature, there were
only some film fragments on the leucosapphire surface covering no more than 40%
of it (Fig. 31.1d).With the annealing temperature increase up to 1600
◦ C, the film
began to disintegrate already after a 2-min exposure (Fig. 31.2); further increase
of annealing time up to 5 min led to a complete decomposition of the film covering
only about 10% of the leucosapphire surface which was almost completely free after
10-min annealing.
489
Annealed samples were examined using scanning electron microscopes JCM6700 and JCM-5000 and an atomic force microscope Nanoscope III A with
micrograph recording. The Raman spectra of titanium and zirconium nanofilms
were obtained using a Renishaw inVia Raman microscope (Renishaw plc, Wottonunder-Edge, UK) at an excitation wavelength of 633 nm.
Using these micrographs, the area of substrate surface coated with metal film
islands was calculated by planimetric weighting method, i.e., by weighting of metalcoated sample parts images cut from micrographs [2]. The data obtained by this
method were analyzed as the dependence of sample surface area covered with metal
film fragments after annealing on annealing parameters (annealing temperature and
time).
31.3 Results and Discussion
Original titanium and zirconium films on both substrates were solid, without any
significant defects, and micrographs obtained using electronic scanning microscopes show only the uniform dark gray field.
During annealing of titanium film on the leucosapphire surface, at first, minor
signs of changes in the structure of the film appeared only as a result of its 2min heating up to 1300
◦ C. As a result of further exposition at this temperature for
5 min, film began to blister in part without losing its integrity, and the process rate is
slightly increased after a 10-min annealing (Fig. 31.1a), but the film still remained
solid. With increased exposition time up to 20 min at 1300
◦ C, the film is rapidly
disintegrated into large pieces. The similar pattern was observed with increase of
annealing temperature up to 1400
◦ C: the film is partially started to blister after
the 2-min exposition without losing its integrity; after a 5-min annealing, process
greatly intensified, and the film even started to crack (Fig. 31.1b). With further
exposition at this temperature for 10 min, quite long and wide cracks appear in the
film; and, finally, after a 20-min annealing, film completely disintegrated into large
fragments between which significant parts of free leucosapphire surface appear.
Annealing at 1500
◦ C has speeded up significantly the process of the titanium
film disintegration. Thus, after the 2-min annealing, film blistered intensively and
lost its integrity; after the 5-min exposition, it is cracked significantly; during
further exposition time increase of up to 10 min, film disintegrated into large
fragments (Fig. 31.1c); and after 2-min annealing at this temperature, there were
only some film fragments on the leucosapphire surface covering no more than 40%
of it (Fig. 31.1d).With the annealing temperature increase up to 1600
◦ C, the film
began to disintegrate already after a 2-min exposure (Fig. 31.2); further increase
of annealing time up to 5 min led to a complete decomposition of the film covering
only about 10% of the leucosapphire surface which was almost completely free after
10-min annealing.