Platinum Sulfide by XPS

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Abstract
It is known from crystallographic investigations that there are two distinct Pt–S modifications, PtS and PtS2 [see R. Collins, R. Kaner, P. Russo, A. Wold, and D. Avignant, Inorg. Chem. 18, 727 (1979); A. Finley, D. Schleich, J. Ackerman, S. Soled, and A. Wold, Mater. Res. Bull. 9, 1655 (1974); S. Soled, A. Wold, and O. Gorochov, ibid. 11, 927 (1976); L. Thomasson, Z. Phys. Chem. Bd. 2, 349; and L. Thomasson, ibid. 4, 277]. They are not commercially available in high grade purity. In the present study the production of pure PtS reference materials and its characterization by x‐ray photoelectron spectroscopy is presented. The PtS2 investigation is shown in a second submission. The PtS samples were produced by annealing stoichiometric mixtures of elemental platinum (DEGUSSA, grade 99.9%) and sulfur (Riedle de Haen, grade 99.5%). Both powders were blended homogeneously and pressed into pellets. The pellets were annealed for 3 weeks in an evacuated quartz tube (800 °C, 10‐4 Pa) and cooled in defined steps to room temperature over 8 days. The materials were investigated by x‐ray diffraction. The diffraction spectrum of PtS agrees with JCPDS 18‐972. This demonstrates the crystalline purity of the reference material. The samples were also characterized by transmission electron microscopy (TEM). The PtS sample consists of isometric particles with sizes between 1 and 3 μm. Selected area diffraction (SAD) and energy dispersive x‐ray spectroscopy (EDXS) give no indication of impurities in the samples.

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