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Understanding Solid‐State Phase‐Formation Processes by Using the High‐Temperature Gas Balance: The Example of Zr 2 PTe 2
Author(s) -
Scholz Tanja,
Schöneich Michael,
Schmidt Peer
Publication year - 2019
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201900281
Subject(s) - chemistry , tellurium , phosphide , ternary operation , solid solution , thermodynamics , solid state , telluride , inorganic chemistry , organic chemistry , nickel , physics , computer science , programming language
Inorganic solid‐state synthesis with phosphorus and tellurium requires a careful control of the reaction parameters because of the high volatility of the components. This initial disadvantage can be used as a benefit for the investigation of phase‐formation mechanisms by analyzing the individual vapor pressure behavior. The high‐temperature gas balance is introduced as a device for detection of heterogeneous solid‐gas equilibria in closed reaction systems. The experimentally challenging synthesis of the phosphide telluride Zr 2 PTe 2 is examined as a model system: optimized synthesis runs at lower temperatures (ϑ = 650 °C) in a faster time, while the quantity as well as the crystalline powder quality is increased. A stepwise solid‐solid reaction of zirconium and tellurium according to Ostwald's rule of stages and the shrinking core model is revealed while phosphorus sublimes and subsequently condenses to react to the ternary compound. Additional phenomena such as melting, expansion, and mechanical instabilities can be observed that broaden the possibilities of the gas balance.