https://arxiv.org/abs/2308.06256

Single crystal synthesis, structure, and magnetism of Pb$_{10-x}$Cu$_x$(PO$_4$)$_6$OThe recent claim of superconductivity above room temperature in Pb$_{10-x}$Cu$_x$(PO$_4$)$_6$O with 0.9 < $x$ < 1 (referred to as LK-99) has sparked considerable interest. To minimize the influence of structural defects and impurity phases on the physical properties, we have synthesized phase-pure single crystals with $x \sim 1$. We find that the crystals are highly insulating and optically transparent. X-ray analysis reveals an uneven distribution of the substituted Cu throughout the sample. Temperature ($T$) dependent magnetization measurements for $ 2 \leq T \leq 800$ K reveal the diamagnetic response characteristic of a non-magnetic insulator, as well as a small ferromagnetic component, possibly originating from frustrated exchange interactions in Cu-rich clusters in the Pb$_{10-x}$Cu$_x$(PO$_4$)$_6$O structure. No anomalies indicative of phase transitions are observed. We therefore rule out the presence of superconductivity in Pb$_{9}$Cu(PO$_4$)$_6$O crystals, and provide some considerations on the origin of anomalies previously reported in experiments on polycrystalline specimen.arxiv.org


https://arxiv.org/abs/2308.05776

On the synthesis methodologies to prepare Pb$_9$Cu(PO$_4$)$_6$O -- phase, composition, magnetic analysis and absence of superconductivityWe present the results of our various attempts to prepare the presumably room-temperature and ambient-pressure superconducting compound Pb$_9$Cu(PO$_4$)$_6$O (LK-99). We experimented with various starting materials, and used several synthesis techniques like, sealed quartz tubes and air-sintering pathways to prepare the reported phase. Repetition of the exact synthesis process followed by Lee et al failed to reproduce the superconducting phase yielding only a multiphase sample. None of our prepared samples exhibits Meissner effect or Levitation. Very importantly, no copper (or only a trace amount) could be detected in any of the designated LK-99 phase with PXRD pattern identical to the reported one. Additionally, some dark greyish flakes in some samples responded towards the magnet in a way imitating half-levitation. The magnetic measurement on those sample suggest it is diamagnetic in the measured temperature range of 2-325 K but show a weak soft ferromagnetic behavior at 2 K, the origin of which is still unknown to us.arxiv.org