The influence of iron on the precipitation behaviour of nickel powder

Journal article

Authors/Editors

Ntuli, Freeman

Research Areas

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Publication Details

Author list: Ntuli F, Lewis AE

Publisher: Elsevier

Place: OXFORD

Publication year: 2007

Journal: Chemical Engineering Science (0009-2509)

Journal acronym: CHEM ENG SCI

Volume number: 62

Issue number: 14

Start page: 3756

End page: 3766

Number of pages: 11

ISSN: 0009-2509

Languages: English-Great Britain (EN-GB)

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Abstract

The effect of iron on the precipitation behaviour of nickel powder was investigated. Reduction experiments were conducted on a 0.5 L laboratory autoclave fitted with a Teflon reaction beaker and a double impeller configuration consisting of an upper axial impeller and lower Rushton turbine. Reduction was conducted in the presence of a morphology modifier at a temperature between 180 and 190 degrees C and 2800 kPa pressure using a synthetic nickel ammine sulphate solution (Ni2+ = 10 g/L, free NH3: Ni2+ and (NH4)(2)SO4: Ni2+ molar ratios of 2.0-2.1 and 2.2, respectively). Nickel seed was used to initiate reduction and iron was added to the reduction solution as ferrous sulphate solution (acidified to pH 2.5 to prevent oxidation) to give a reduction solution with Fe2+ concentration of 6, 20 and 200 mg/L. The effect of iron was investigated by studying the evolution of the moments, volume or mass moment mean D(4.3), number based mean size ((L) over bar (1.0)), nickel depletion rate and population balance in the absence of sampling between batch reductions. Iron was found to act as a growth promoter and nucleation agent through reversible adsorption and hydrolysis on the surface of the seed particles. Growth was preferentially favoured over nucleation up to a Fe2+ concentration of 6 mg/L, thereafter the extent of nucleation increased with increasing Fe2+ concentration up to 200 mg/L. Nucleation and growth promotion in the presence of high shear rates gave rise to rapid aggregation, which ceased at a critical size of approximately (L) over bar (1.0) = 10 mu m and D(4.3) = 66 mu m in the presence of iron and (L) over bar (1.0) = 15 mu m without. However, the sharp increase in the D(4.3) towards the end of the cycle and the general decrease in surface area shows that aggregation of larger particles plays a major role in size enlargement. Comparison of the scanning electron microscopy (SEM) micrographs of the powder with undesirable morphology produced in industrial practice and that produced in the laboratory in the presence of iron showed that iron was one of the factors responsible for the production of powder with undesirable morphology. Based on these laboratory scale experiments, iron levels in reduction solutions should not exceed 6 mg/L for effective control of particle morphology. (c) 2007 Elsevier Ltd. All rights reserved.

Keywords

crystallisation, impurity, Iron, Nickel reduction, Particle formation, Precipitation

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