HYDROGEN REDUCTION

The production of metal powders by

hydrogen reduction of compounds or
solutions has been investigated in recent
years by numerous authors. Fine metal
powders gained increasing relevance for
sophisticated materials. Powders with
grain sizes below 1 m for magnetic
materials, catalysts,andchemicalsensors
are of great importance for many industries.
Such powders cannot be obtained
by simple processes like milling or
atomization.Thereductionofcompounds
(e.g., oxides and chlorides) and also of
solutions by hydrogen exhibit a possible
alternative for the synthesis of fine metal
powders. This technology is state of the
art for the production of tungsten and
molybdenum powders, and it is being
considered for application for the manufacture
of other metal powders.
Furthermore, the reduction by hydrogen
enables the production of ultra-pure
metals with high yields (>99%). The
content of impurities only amounts to
4060 ppm if appropriate pure oxides
are applied. Such high-purity metals are
often required as targets or as reference
materials.

At higher temperature and pressure, hydrogen can lead to the precipitation of metals
or oxides.
Metals like cobalt (Co), nickel (Ni), copper (Cu), iron (Fe), and uranium dioxide (UO 2)
are precipitated on the industrial scale using the method of hydrogen reduction.
The reduction is carried out in the horizontal stainless steel autoclaves equipped with
the agitators, baffles, heating or cooling coils, and the necessary connection for the
feed and gas inlet and outlet.
The production of this technique is a highly-purity power that can be used as such, or
in case of metals, hot pressed and rolled in form of strips.
Precipitation may be conducted from aqueous as well as non-aqueous media.
Precipitation of metals from aqueous media:
Reaction: M2+ + H2

M + 2H+

The equilibrium constant is:

Kc = [H+]2 [M2+] PH2

The precipitation of copper (Co) from CuSO 4 solution takes place through the
disproportionation of cuprous ion which has identified in the course of reaction:
2Cu2+ +H2 = 2Cu2+ + 2H+
2Cu+ = Cu + Cu2+
The reaction results in lowering the yield of the metal, which results in depositing
more metals if hydrogen ion is removed as soon as they are formed. For cobalt (Co),
nickel (Ni), copper (Cu), this is conveniently done by the operating in ammoniacal
medium.
Reaction:

[M (NH3)n]2+ = nNH3 + M2+

M2+ + H2 = M + 2H+
H+ + NH3 = NH4+

Increasing the ammonia concentration has two opposing effects:

Precipitation is favoured due to the neutralization of the liberated acid

Precipitation is hindered because of the decrease in the reducible metal ion
(M+) due to the complexing action.

The amount of the ammonia in the solution influences the rate of the precipitation.
The rate of precipitation in cobalt (Co) achieves the maximum when [NH 3] / [Co2+].
The removal of hydrogen ion when they are formed in the reduction is done by
reducing hydroxide (OH-) slurries.
Equations:

M(OH)2 = M2+ + 2OHM2+ + H2 = M + 2H+

OH- + H+ = H2O

Overall reaction:

M(OH)2 + H2 = M + H2O

The reaction of cobalt (Co) and nickel (Ni) take place at higher temperature of
270C, and the product is of extremely fine particle size.