Molybdenum oxygen-containing solid-phase compounds were electrodeposited on the platinum cathode from the alkaline solutions containing sodium molybdate or ammonium molybdate under galvanostatic condition.
Bath composition and electrolytic condition were as follows:
Sodium bath: Na
2MoO
4·E
2H
2O (0.2M), NaOH (for adjusting pH10.5)
Ammonium bath:(NH
4)
6Mo
7O
24·E
4H
2O (0.2M as Mo), NH
4OH (for adjusting pH10.5)
Current density: 50mA/cm
2, Temperature: 70°C
Black deposits were obtained from the sodium baths and black-brown deposits from the ammonium baths.
Structure of these deposits were investigated by studying the crystallization processes of the deposits. Thermal analysis curves, X-ray diffraction pattern, infra-red absorption spectra measurements and trymethyl-silylation of the deposits were carried out and following results were obtained.
As plated state, deposits were amorphous MoO
2-n (OH)
2n (n; 0-2). Deposits obtained from the sodium bath contained Mo
6+and Na+. Deposits were dehydrated to crystallize as MoO
2, Na
2Mo
3O6.5 and small amount of Na
2MoO
4 with elevating temperature.
Deposits obtained from the ammonium bath contained NH4. Differing from the deposits obtained from the sodium bath, they scarcely contained Mo
6+. Deposits dehydrated with vapouring NH
3 to crystallize as MoO
2 by elevating temperature.
抄録全体を表示