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La2CuO4+δ: Synthesis under high oxygen pressure and study of phase relations and energetics

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Abstract

High oxygen pressures have been achieved in a piston-cylinder apparatus using a double capsule assembly consisting of a sealed outer Au capsule, containing an oxygen source (KMnO4), and an inner, open Pt capsule containing the sample. Using this technique, La2CuO4 was annealed at 800 °C, 5–25 kbar for 2–4 h. Transposed temperature drop calorimetry at 704 °C was used to determine the enthalpy of oxidation, and weight loss measurements characterized the oxygen nonstoichiometry, δ, in La2CuO4+δ, in the high-pressure, oxygen-annealed samples. For samples analyzed at room temperature, x-ray diffraction measurements show that beyond δ ≍ 0.10–0.13, additional oxygen is accommodated in a perovskite-like LaCuO3−α phase. An analysis of the thermochemical measurements indicates that the nature of holes in La2CuO4+δ could change in the range of δ ≍ 0.03–0.06.16,17 It is further suggested that the observed change in the thermochemical behavior in the range of δ ≍ 0.03–0.06 could be the driving influence behind the spinodal decomposition of La2CuO4+δ at low temperatures (Dabrowski et al.10).

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Authors and Affiliations

  1. Department of Geological and Geophysical Sciences and Princeton Materials Institute, Princeton University, Princeton, New Jersey, 08544-1003, USA

    R. P. Rapp, A. Mehta, J. DiCarlo & A. Navrotsky

  2. Center for High Pressure Research, an NSF Science and Technology Center, Princeton University, Princeton, New Jersey, 08544-1003, USA

    R. P. Rapp & A. Navrotsky

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  1. R. P. Rapp
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  2. A. Mehta
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  3. J. DiCarlo
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  4. A. Navrotsky
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Rapp, R.P., Mehta, A., DiCarlo, J. et al. La2CuO4+δ: Synthesis under high oxygen pressure and study of phase relations and energetics. Journal of Materials Research 9, 8–12 (1994). https://doi.org/10.1557/JMR.1994.0008

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  • DOI: https://doi.org/10.1557/JMR.1994.0008

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