The Al–Fe–Si system was studied for an isothermal section at 800 °C in the Al-rich part and at 900 °C in the Fe-rich part, and for half a dozen vertical sections at 27, 35, 40, 50 and 60 at.% Fe and 5 at.% Al. Optical microscopy and powder X-ray diffraction (XRD) was used for initial sample characterization, and Electron Probe Microanalysis (EPMA) and Scanning Electron Microscopy (SEM) of the annealed samples was used to determine the exact phase compositions. Thermal reactions were studied by Differential Thermal Analysis (DTA). Our experimental results are generally in good agreement with the most recent phase diagram versions of the system Al–Fe–Si. A new ternary high-temperature phase τ12 (cF96, NiTi2-type) with the composition Al48Fe36Si16 was discovered and was structurally characterized by means of single-crystal and powder XRD. The variation of the lattice parameters of the triclinic phase τ1 with the composition Al2+xFe3Si3−x (−0.3 < x < 1.3) was studied in detail. For the binary phase FeSi2 only small solubility of Al was found in the low-temperature modification LT-FeSi2 (ζβ) but significant solubility in the high-temperature modification HT-FeSi2 (ζα) (8.5 at.% Al). It was found that the high-temperature modification of FeSi2 is stabilized down to much lower temperature in the ternary, confirming earlier literature suggestions on this issue. DTA results in four selected vertical sections were compared with calculated sections based on a recent CALPHAD assessment. The deviations of liquidus values are significant suggesting the need for improvement of the thermodynamic models.

The quaternary system Al–Fe–Si–Ti was studied in the iron-rich corner for sections at 50, 60 and 70 at.% Fe at 900 °C. Isothermal phase equilibria were investigated by a combination of optical microscopy, X-ray powder diffraction (XRD) followed by Rietveld refinement and Electron Probe Microanalysis (EPMA). Phase boundaries of the phases, in particular of the Laves phase (Fe2Ti) and of the extended phase field of A2/B2/D03, were investigated. Selected samples containing the Laves phase and the B2 phase were characterized by microhardness measurements at different compositions throughout the quaternary homogeneity range of the phases.

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A study of the ternary Rh–Mn–Bi phase diagram revealed the existence of two new ternary bis­muthides, viz. hexa­rhodium penta­manganese octadecabismuthide (Rh6Mn5Bi18) and rhodium manganese tribismuthide (RhMnBi3). Their crystal structures represent new structure types.