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PhD Thesis_RuiMSMartins.pdf - RUN UNL

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In-situ XRD studies during growth of Ni-Ti SMA films and their complementary ex-situ characterization<br />

concomitant high ion flux. A characteristic of this source discharge is a column of plasma,<br />

which leaves the magnetic tunnel region and projects normal to the target surface towards the<br />

substrate position. In consequence, a large flux of charged particles (electrons and ions)<br />

reaches the substrate and, by suitable biasing, the energy of ions impinging on the growing<br />

film can be varied. The micrographs have shown that the microstructure of the films was<br />

influenced by the degree of ion bombardment (V b ). The increase in ion energy by applying a<br />

V b of −45 V led to apparently larger crystals in the form of regular polyhedron visible on the<br />

surface of the film. A further increase of V b to −90 V led to the appearance of surface steps on<br />

the crystals morphology.<br />

The results presented in this section have shown that a TiN buffer layer acts not only<br />

as a diffusion barrier, but there is also a relationship between the TiN substrates and Ni-Ti<br />

texture development (B2 phase):<br />

1) there was a preferential growth of oriented grains of the Ni-Ti B2 phase<br />

from the beginning of the deposition, with a constant growth rate during the whole<br />

deposition, for a Ni-Ti film deposited (without and with V b of −45 and −90V) on<br />

TiN with a topmost layer formed mainly by oriented grains;<br />

2) in the case of Ni-Ti films deposited on top of a TiN layer where a dominating<br />

orientation could not be identified (primarily, and oriented grains of<br />

TiN nucleate and grow), a different behaviour was observed;<br />

- without V b applied, oriented grains of the Ni-Ti B2 phase dominated at<br />

lower thickness values, while, oriented grains took over at higher<br />

thickness values.<br />

- with V b of −45V, the development of the oriented grains of the Ni-Ti<br />

B2 was reduced and the oriented grains dominated since the beginning.<br />

According to the ER results obtained during temperature cycling, the distinct<br />

crystallographic orientations of the Ni-Ti films influence their phase transformation<br />

characteristics. The resistivity increase during R-phase transformation, on cooling and<br />

heating, was higher for Ni-Ti films with a higher fraction of grains of the B2 phase with (211)<br />

parallel to the film surface. The ER measurements have also shown that for the deposition of<br />

Ni-Ti films with V b (−45 and −90 V), the transformation temperatures of the various phases<br />

were shifted to lower values, when compared with the depositions performed without<br />

applying V b .<br />

Chapter 3 – Results 138

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