Pure aluminum specimens were covered with hydrous oxide films by immersion in boiling distilled water and then anodized galvanostatically in a neutral borate solution at different temperatures to form composite oxide films. The formation behavior of the hydrous oxide and composite oxide films was examined by gravimetry, XPS, chemical analysis and electron microscopy.
It was found that the hydrous oxide films consist of two layers; a fibrous outer layer (thickness δ
h.o) and a dense inner layer (δ
h.i). The thickness of the outer layer, δ
h.o, increased rapidly with time to reach a steady value of ca. 0.3μm but that of the inner layer, δ
h.i, continued to increase gradually after a rapid increase. The hydrous oxide had a chemical composition of Al
2O
3⋅2.7H
2O and a density of ca. 2.3g/cm
3, both of which did not change with immersion time.
The composite oxide films consisted of two layers; an outer crystalline oxide layer (thickness δ
o) and an inner amorphous oxide layer (δ
i). During anodizing, δ
h.i decreased linearly, and the total thickness, δ
o+δ
i, increased linearly with
ta. The δ
h.i vs.
ta and δ
o+δ
i vs.
ta curves were independent of anodizing temperature,
Ta. The outer layer thickness, δ
o, increased with
ta, at a rate increasing with
ta. This behavior was pronounced at higher
Ta. The rate of increase in δ
i decreased with
ta, and this also became more pronounced at higher
Ta. The electric field supported by δ
i+δ
o was found to increase with
ta from 7.7 to 10.3×10
6V/cm. This is explained as being due to the formation of the crystalline oxide layer capable of supporting higher electrical field and to the increase in δ
o/(δ
i+δ
o).
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