Hydrothermal synthesis and physicochemical characterization of CuO/ZnO/Al2O3 nanopowder. Part I: Effect of crystallization time--颗粒学报PARTICUOLOGY

Saedy, S., Haghighi, M., & Amirkhosrow, M. (2012). Hydrothermal synthesis and physicochemical characterization of CuO/ZnO/Al2O3 nanopowder. Part I: Effect of crystallization time. Particuology, 10(6), 729–736. https://doi.org/10.1016/j.partic.2012.05.001

Hydrothermal synthesis and physicochemical characterization of CuO/ZnO/Al₂O₃ nanopowder. Part I: Effect of crystallization time

Saeed Saedy^{a b}, Mohammad Haghighi ^{a b *}, Mahsa Amirkhosrow ^{a b}

a Chemical Engineering Department, Sahand University of Technology, P.O. Box 51335-1996, Sahand New Town, Tabriz, Iran
b Reactor and Catalysis Research Center, Sahand University of Technology, P.O. Box 51335-1996, Sahand New Town, Tabriz, Iran

10.1016/j.partic.2012.05.001

Volume 10, Issue 6, December 2012, Pages 729-736

Received 23 December 2011, Revised 21 April 2012, Accepted 3 May 2012, Available online 19 July 2012.

E-mail: haghighi@sut.ac.ir

Highlights

► CuO/ZnO/Al₂O₃ (CZA) nanopowder was synthesized hydrothermally with atomic ratio of 6:3:1.

► Relative crystallinity increased with increasing crystallization time.

► The optimal crystallization time is 6 h with crystallite size of 20 nm.

► EDX mapping indicated homogenous dispersion of elements.

Abstract

A hydrothermal method was successfully used for synthesis of CuO/ZnO/Al₂O₃ (CZA) nanopowder with atomic ratio of 6:3:1. The effect of crystallization time (3, 6, 9, and 12 h) on physicochemical properties of nanopowder was investigated. Nanopowders were characterized using XRD, FESEM, EDX, FTIR, TG, and BET techniques. The XRD patterns confirmed metal oxides formation and their good crystallinity with average crystallite size of 20 nm as obtained by the Scherrer equation. Relative crystallinity was shown to increase with increasing crystallization time. In agreement with XRD results, FESEM images also illustrated nanosized particles. EDX mapping indicated homogenous dispersion of elements. BET specific surface area analysis showed acceptable surface area for CZA nanopowder. FTIR spectroscopy confirmed metal oxides formation during hydrothermal and calcination processing. TG results illustrated high thermal stability of the synthesized nanopowders. TG-DTG and FTIR analyses were used to propose a reaction mechanism for nanopowder formation during processing. Physicochemical characterization showed optimal crystallization time to be 6 h.

Graphical abstract

Keywords

ZnO; CuO; Al₂O₃; Mixed oxides; Nanopowder; Hydrothermal

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