The formation of a bi-layer coating consisting of Ni aluminide/Ni-Hf alloy on a Ni substrate was attempted by the electrodeposition of Hf on the Ni substrate, followed by the electrodeposition of Ni and Al. Before the formation of this coating, it was confirmed by the diffusion couple test that the Ni-Hf alloy consisting of Ni
7Hf
2 acted as a diffusion barrier of aluminum. Upon forming this bi-layer coating, Hf and Al were deposited by molten salt electrolysis at 1023 K. The cyclic oxidation resistance for the Ni covered with this coating was then evaluated in air at 1373 K. The electrodeposition of Hf on the Ni substrate led to the formation of a layer consisting of the Ni-Hf alloy. The electrodeposition of Ni and Al on the Ni-Hf alloy layer led to the formation of a layer consisting of Ni
2Al
3 as a surface layer. The cyclic oxidation test showed that the mass gain due to oxidation for the sample covered with the bi-layer coating consisting of the Ni
2Al
3/Ni-Hf alloy was lower than that for the sample covered with a single-layer coating consisting of Ni
2Al
3. The analytical results of a cross-section of the sample covered with the bi-layer coating after the 5-cycle oxidation test showed that the chemical composition of the Ni-Hf alloy layer was uniform, and this layer consisted of Ni
7Hf
2. Furthermore, it was confirmed that the aluminum concentration in the Ni aluminide layer was constant at about 40 at%, and the Ni-Hf alloy layer depressed the diffusion of aluminum from the Ni aluminide layer to the Ni substrate. For the sample covered with the bi-layer coating after the 100-cycle oxidation test, the aluminum concentration in the Ni aluminide layer was constant at about 20 at%, and a protective alumina scale containing small amounts of hafnium oxide was formed. On the contrary, for the sample covered with the single-layer coating consisting of Ni
2Al
3, the aluminum concentration in the Ni aluminide layer was only about 10 at%, and an internal oxide was largely formed in the Ni aluminide layer.
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