Potential and limitations of microanalysis SEM techniques to characterize borides in brazed Ni-based superalloys

• We attempt to accurately identify Boron-rich phases in Ni-based superalloys.
• EDS, WDS, EBSD systems are tested for accurate identification of these borides.
• Results are compared with those obtained by electron probe microanalysis.
• Boron was measured with EDS by composition difference with a precision of 5 at. %.
• Additional EBSD in phase identification mode conclusively identifies the borides.

Brazed Ni-based superalloys containing complex phases of different Boron contents remain difficult to characterize at the micrometer scale. Indeed Boron is a light element difficult to measure precisely. The state-of-the-art microanalysis systems have been tested on a single crystal MC2 based metal brazed with BNi-2 alloy to identify boride precipitates. Effort has been made to evaluate the accuracy in Boron quantitation. Energy-dispersive and wavelength-dispersive X-ray spectroscopy attached to a Scanning Electron Microscope have first been used to determine the elemental composition of Boron-free phases, and then applied to various types of borides. Results have been compared to the ones obtained using a dedicated electron probe microanalysis, considered here as the reference technique. The most accurate method to quantify Boron using EDS is definitely by composition difference. A precision of 5 at.% could be achieved with optimized data acquisition and post-processing schemes. Attempts that aimed at directly quantifying Boron with various standards using EDS or coupled EDS/WDS gave less accurate results. Ultimately, Electron Backscatter Diffraction combined with localized EDS analysis has proved invaluable in conclusively identifying micrometer sized boride precipitates; thus further improving the characterization of brazed Ni-based superalloys.