Silver electrodes were studied by means of potentials and x‐ray diffraction patterns. The silver was charged anodically in
35%KOH
by means of either constant current or constant potential, and discharged at a low or high rate. Attempts were made to form an oxide higher than
normalAgO
by means of anodization. The products of anodization of silver in
2N H2SO4
were determined. The basis for the theory that the oxides of silver are formed by the introduction of oxygen into the octants of the face‐centered cubic silver lattice was examined.
Silver electrodes were examined in 20–50%
KOH
using a cell permitting simultaneous x‐ray diffraction and electrochemical studies. Highly oriented smooth rolled sheet Ag developed randomly oriented Ag on its surface during early cycles. Charge‐discharge capacity increased to a maximum as surface area increased.
normalAgO
crystal size and amount formed varied inversely with charging c. d. High charge rates gave tight coatings of small
normalAgO
crystals that limited further oxidation. Reactions took place initially at the outer surface of the electrode. Oxidation to
Ag2O
and
normalAgO
and reduction to
Ag2O
and Ag occurred by formation of distinct crystals rather than expansion or contraction of preexisting crystal lattices. Discharge capacity at the
normalAgO/Ag2O
potential plateau depended more on surface area than on quantity of
normalAgO
. A slow discharge produced smoother Ag surfaces, lowering capacity of the next cycle. There was never evidence of a suboxide, oxidation state higher than
normalAgO
, solid solution, or alloy of oxygen and silver.
The anodic corrosion product formed on lead in sulfuric acid solutions depends on the potential of the metal surface.In the potential range between lead-lead sulfate and lead sulfate-lead dioxide, the following compounds were identified by electron diffraction: monobasic lead sulfate, lead hydroxide, and lead monoxide. In additibn, the diffraction pattern for an unidentified material was observed. Coordinated potential-time curves show arrests corresponding to the appearance of these compounds. The physical nature of these corrosion films is discussed.
normalPbO·PbSO4
,
3normalPbO·PbSO4·H2O
, and
4normalPbO·PbSO4
were prepared by reacting
normalPbO
and dilute
H2SO4
. The crystalline phases were identified by x‐ray diffraction patterns, and electron microscope examination showed all three to be prismatic needles, The three basic sulfates were oxidized anodically in dilute sulfuric acid, and x‐ray diffraction showed that each transformed to
βPbO2
. The pellet made from
4normalPbO·PbSO4
was mechanically strong, and the transformation to
PbO2
was largely metasomatic after the original crystals of the basic sulfate. The three anodic preparations were examined in the electron microscope and showed the presence of prismatic and nodular particles of
PbO2
.
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