Polymorph selectivity of superconducting CuSe₂ through kinetic control of solid-state metathesis

Journal of the American Chemical Society
Andrew J MartinolichJames R Neilson

Abstract

Rational preparation of materials by design is a major goal of inorganic, solid-state, and materials chemists alike. Oftentimes, the use of nonmetallurgical reactions (e.g., chalcogenide fluxes, hydrothermal syntheses, and in this case solid-state metathesis) alters the thermodynamic driving force of the reaction and allows new, refractory, or otherwise energetically unfavorable materials to form under softer conditions. Taking this a step further, alteration of a metathesis reaction pathway can result in either the formation of the equilibrium marcasite polymorph (by stringent exclusion of air) or the kinetically controlled formation of the high-pressure pyrite polymorph of CuSe2 (by exposure to air). From analysis of the reaction coordinate with in situ synchrotron X-ray diffraction and pair distribution function analysis as well as differential scanning calorimetry, it is clear that the air-exposed reaction proceeds via slight, endothermic rearrangements of crystalline intermediates to form pyrite, which is attributed to partial solvation of the reaction from atmospheric humidity. In contrast, the air-free reaction proceeds via a significant exothermic process to form marcasite. Decoupling the formation of NaCl from the form...Continue Reading

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Oct 15, 2014·Journal of the American Chemical Society·Andrew J Martinolich, James R Neilson
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Nov 15, 2014·Inorganic Chemistry·Sergio ConejerosEnric Canadell

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Citations

Aug 5, 2016·Journal of the American Chemical Society·Andrew J MartinolichJames R Neilson
Jun 2, 2017·Chemical Science·A M BelenguerJ K M Sanders
Jul 15, 2020·Chemical Communications : Chem Comm·Paul K ToddJames R Neilson
Sep 10, 2016·Journal of Physics. Condensed Matter : an Institute of Physics Journal·C Stock, E E McCabe
Apr 30, 2021·Inorganic Chemistry·Marcela CalpaKiyoharu Tadanaga
Jan 10, 2019·Journal of the American Chemical Society·Paul K Todd, James R Neilson
Aug 22, 2017·Accounts of Chemical Research·Min-Rui GaoShu-Hong Yu

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