In order to improve hydrogen absorption and desorption rates, an ion-plating method was applied to the plating of Pd and Ni onto Ta and Nb specimens and the optimum conditions were determined. The structure and properties of the ion-plated films for various plating conditions and some problems connected with hydrogen absorption-desorption cycles were also investigated.
The results obtained are summarized as follows:
(1) From the Auger experiment, the surface of Nb as emery polished is covered by equal amounts of oxygen and carbon and a clean surface was obtained by 120 s sputter-etching (2 nm sputter depth).
(2) As for the argon glow-discharge sputter-etching, we have observed critical values for the discharge voltage at which the sputter-yield becomes approximately zero. The values depended strongly on the purity of argon used and were ∼600 V for Nb and ∼400 V for Ta under purified argon (10
−6 ppm O
2) and ∼1.8 kV for Nb and ∼1.5 kV for Ta under commercial argon (10 ppm O
2).
(3) The scanning electron microscopic observation showed that the films have a columnar structure and there are no significant differences among those under different plating conditions (discharge voltage 0.5∼3.8 kV, Ar pressure 1.3∼8.0 Pa and electric power 3∼30 W).
(4) In many cases, exfoliation of the films occurred in the vicinity of the brittle intermediate phases (NbPd
3, NbNi
3 etc.), which were formed by the heat treatment around 1170 K.
(5) When Pd ion-plated Nb was subjected to the hydrogen absorption-desorption cycles under 573 K, hydrogen induced rupture of the Nb specimen occurred. Even in this case, the Pd film did not exfoliate from the substrate.
(6) The hydrogen absorption rate of Pd ion-plated Nb deteriorated remarkably after the absorption-desorption cycles at 873∼1173 K. In this case, adsorption of carbon and oxygen onto Nb diffused to the surface of the Pd film was observed.
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