Formation of Cu₂SnSe₃ from stacked elemental layers investigated by combined in situ X-ray diffraction and differential scanning calorimetry techniques

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• 作者：Rachmat Adhi Wibowo ; Stefan Moeckel ; Hyesun Yoo ; Astrid Hoelzing ; Rainer Hock ; Peter J. Wellmann
• 关键词：Intermetallics ; Thermoelectric materials ; Solid state reactions ; Phase transitions
• 刊名：Journal of Alloys and Compounds
• 出版年：5 March, 2014
• 年：2014
• 卷：588
• 期：Complete
• 页码：254-258
• 全文大小：926 K

文摘

Stacked elemental layers of Mo/Cu/Sn and Mo/Cu/Sn/Se were employed as samples for investigating the formation reaction of Cu-Sn intermetallic compounds as well as Cu₂SnSe₃ phases by in situ technique of X-ray diffraction and differential scanning calorimetry. The use of a combined in situ technique allows a real-time observation on solid-state reactions as well as any crystalline phase changes during annealing towards the crystallization of Cu₂SnSe₃. It is found that Cu and Sn form intermetallic compounds of Cu₆Sn₅, Cu₃Sn and Cu₄₁Sn₁₁ as the annealing temperature rises from 30 to 550 掳C. The reaction of Se with Cu to form a CuSe phase dominates the binary phase formation at a low annealing temperature. The annealing of a stacked Mo/Cu/Sn/Se layer suggests that only Cu₆Sn₅ intermetallic compound directly acts as a reactant for the Cu-selenide phase formation. A SnSe phase mostly forms from a liquid-state reaction of Sn and Se above the Sn melting point. The in situ investigation also reveals a complete set of Cu-selenide peritectic decompositions of CuSe₂ 鈫?#xA0;CuSe 鈫?#xA0;Cu_1.8Se at 360 and 412 掳C. The formation of Cu₂SnSe₃ phase starts at 450 掳C as a product from a reaction between Cu_1.8Se and SnSe in a presence of liquid Se. Comparisons on the initial formation temperatures of all involved phases and on the formation pathways between Cu₂SnSe₃ and Cu₂SnS₃ are discussed as well.