Identification of solid solutions of coprecipitated Ni-Co oxalates using XRD, TG and SEM techniques

doi:10.1016/0040-6031(93)80456-K

Thermochimica Acta

Volume 220, June 1993, Pages 75-89

https://doi.org/10.1016/0040-6031(93)80456-K Get rights and content

Abstract

Homogeneous solid-solution oxalates of Ni²⁺ and Co²⁺ ions were synthesized by coprecipitation from nitrate solutions using a double-inlet technique. The identification of the solid solutions used X-ray powder diffraction (XRD), thermogravimetry (TG) and scanning electron microscopy (SEM) techniques. The experimental results showed that the coprecipitated powders have characteristics that are different from those of the mechanical mixtures with the same stoichiometry.

References (13)

H. Langbein et al.
Thermochim. Acta
(1991)
D. Dollimore
Thermochim. Acta
(1991)
A. Inzenhofer
Sprechsaal
(1985)
H. Hausner
Ber. Dtsch. Keram. Ges.
(1978)
G. Tomanndl et al.
Ber. Dtsch. Keram. Ges.
(1985)
D.G. Wickham
Inorg. Synth.
(1967)

There are more references available in the full text version of this article.

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The coprecipitates Ag₂Zn_1−xNi_x(OX)₂·2H₂O (x=0.3, 0.5, 0.7, and ox=oxalate anion) and Ag₂Zn_0.5Co_0.5(OX)₂·2H₂O have been prepared and characterized by means of infrared spectroscopy (IR), elemental analysis, X-ray powder diffractometry (XRD), scanning electron microscopy (SEM) and thermal analyses (DTA/TG). The results indicate, that the coprecipitates are solid solutions. The thermal decomposition of the compounds in both dynamic and static air has been studied. The study also showed that the water of crystallization practice different interactions in the lattice of the solid solutions. The thermal decomposition products of the coprecipitates in static air were investigated by IR, XRD and SEM. The electrical conductivity of the final mixed oxides in static air was also measured.

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Regular papersIdentification of solid solutions of coprecipitated Ni-Co oxalates using XRD, TG and SEM techniques

Abstract

Thermochim. Acta

Thermochim. Acta

Sprechsaal

Ber. Dtsch. Keram. Ges.

Ber. Dtsch. Keram. Ges.

Inorg. Synth.

Regular papers
Identification of solid solutions of coprecipitated Ni-Co oxalates using XRD, TG and SEM techniques