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Quantitative analysis of morphology of polycrystalline precipitate received in temperature ranges of growth rate anomalies

Liubov A. Khazikova 1Sergey N. Bocharov 2

1. Saint-Petersburg State University, Saint-Petersburg, Russian Federation
2. Saint-Petersburg State University (SPBSU), 7/9 University emb., S.Petersburg 199034, Russian Federation

Abstract

Kinetic anomalies were discovered in 1967 and were found in all detailed measurements in randomly selected systems [3]. Anomalies represent the temperature ranges in which the growth rate undergoes sharp changes. It was subsequently shown that anomalies have a significant influence on kinetic dependent properties of crystals such as chemical composition [1] and morphology [2]. Influence of kinetic anomalies on crystals morphology was investigated only for single crystals and at quality level. So the aim of this work is study of polycrystalline deposit morphology in the temperature range of kinetic anomalies.

Investigation of polycrystalline precipitate morphology in dependence on temperature was performed at copper electrocrystallization as example.  The experiments were carried out in a temperature range of 46.0-51.0 ° C in solution of copper sulphate with a fixed concentration 15 g of the salt per 100 g of water.  Kinetic curve for this temperature range and concentration was obtained earlier and it reproduces kinetic curve known from the reference [4]. Electrochemical copper precipitate obtained at different temperatures has been studied ex-situ by atomic force microscopy with quantitative analysis of received AFM images. Quantitative analysis consisted in statistical processing of images of the surface morphology in the NOVA program. We took the following characteristics as the main parameters that characterize morphology of the deposit: average roughness, scale height, ten point height, deviation from the mean height.

Statistical characteristics of copper precipitate morphology in dependence on temperature vary non monotonically. These variations have the same  temperature positions but intensities are different that what we relate to the method of curves normalization.  Quantitative characteristics of copper precipitate morphology reproduce kinetic curve of copper electrocrystallization in dependence on temperature. It confirms the data on kinetic anomalies influence on crystal morphology obtained for monocrystals case.

References:

 [1] A.A. Chernov, V.V. Sipyagin, Current Topics in Materials Science, 5, p. 281 (1980).

[2] S. N. Bocharov, P. Gille,  A. E. Glikin, Cryst. Res. Technol., 44, 1, p. 13 (2009).

[3]A.E. Glikin, S.N. Bocharov, E.V. Kir’yanova, V.V. Sipyagin, Zap. Vseross. Mineral. O–va, No. 2, p.99 (2003) [in Russian].

[4] S.N. Bocharov, A.E. Glikin, Crystallography Reports, Vol. 53, 1, p. 147 (2008).

 

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Related papers

Presentation: Poster at 17th International Conference on Crystal Growth and Epitaxy - ICCGE-17, General Session 1, by Liubov A. Khazikova
See On-line Journal of 17th International Conference on Crystal Growth and Epitaxy - ICCGE-17

Submitted: 2013-04-15 21:30
Revised:   2013-05-14 13:02