Effect of thermal processing on the microstructure and composition of Cu–Sb–Se compounds

• Published in: Journal of materials science Vol. 48; no. 5; pp. 2188 - 2198
• Main Authors: Majsztrik, P. W., Kirkham, M., Garcia-Negron, V., Lara-Curzio, Edgar, Skoug, E. J., Morelli, D. T.
• Format: Journal Article
• Language: English
• Published: Boston Springer US 01.03.2013; Springer; Springer Nature B.V
• Subjects: Annealing; Characterization and Evaluation of Materials; Chemistry and Materials Science; Classical Mechanics; Composition; Cooling; Copper; Copper selenides; Crystallography and Scattering Methods; Diffusion rate; Materials Science; Microstructure; Modulus of elasticity; Nanoindentation; Polymer Sciences; Solid Mechanics; Stoichiometry; Thermoelectric Material; CuInSe; Peritectic Reaction; Ternary Phase Diagram; Cu2Se
• ISSN: 0022-2461; 1573-4803
• DOI: 10.1007/s10853-012-6994-x

We report on the effects of thermal processing on the microstructure and composition of a system with overall stoichiometry of 3Cu:1Sb:3Se with the aim of producing single-phase Cu 3 SbSe 3 . It was found that slow cooling from the melt produced a multiphase material consisting of Cu 2 Se and CuSbSe 2 , but devoid of Cu 3 SbSe 3 . Cooling rapidly from the melt resulted in three-phase microstructures consisting of Cu 2 Se, CuSbSe 2 , and Cu 3 SbSe 3 . Subsequent annealing of the three-phase material between 325 and 400 °C shifted the composition toward nearly pure Cu 3 SbSe 3 —the target compound of this work. The kinetics of the transformation into Cu 3 SbSe 3 was successfully described using a modified Avrami model which suggests that diffusion is the rate-controlling step. Values of Young’s modulus and hardness, obtained by nanoindentation, are reported for Cu 2 Se, CuSbSe 2 , and Cu 3 SbSe 3 .