Letters to Nature

Nature 389, 164-167 (11 September 1997) | doi:10.1038/38249; Received 26 March 1997; Accepted 8 July 1997

Application of scanning SQUID petrology to high-pressure materials science

Bruce A. Scott1,2, John R. Kirtley2, David Walker1, Bai-Hao Chen1 and Yanhui Wang1

  1. Lamont-Doherty Earth Observatory of Colombia University, Palisades, New York 10964, USA
  2. IBM Thomas J. Watson Research Center, Yorktown Heights, New York 10598, USA

Correspondence to: Bruce A. Scott1,2 Correspondence and requests for materials should be addressed to B.A.S. (Email: scottba@watson.ibm.com).

High-pressure synthesis is increasingly being used in the search for new materials. This is particularly the case for superconductors1, but the synthesis products are difficult to analyse because they are small in size (approx50 mg) and often consist of a mixture of unknown phases exhibiting a low superconducting volume fraction. X-ray or electron diffraction cannot identify a superconductor unambiguously if it is a minority constituent. Here we report a methodology—'scanning SQUID petrology'—that combines the use of a scanning SQUID microscope2 with petrological techniques to image and identify low concentrations of superconducting phases in complex phase assemblages. We demonstrate the power of this methodology by investigating the poorly understood origin of superconductivity in the high-pressure Sr–Cu–O system1. A Sr2CuO3 + KClO3 diffusion couple3 processed at 60 kbar and 950 °C yielded the superconductor Sr3Cu2O5Cl at the approx3% level adjacent to the oxidizer. In addition to the unexpected participation of chlorine from an ostensibly 'inert' oxidizer that is commonly used in high-pressure synthesis work, the sample was highly zoned owing to limited oxygen diffusion kinetics, and contained non-superconducting Sr2CuO3.2. These contamination and diffusion problems probably affected all previous high-pressure copper oxide diffusion-couple experiments. Scanning SQUID petrology has general applicability to heterogeneous samples and is capable of detecting magnetic or superconducting phases at concentrations of less than 1 p.p.m.