Validation and traceability of XRF and SEM‐EDS elemental analysis results for solder in high‐reliability applications

A procedure and calibration samples were developed for X‐ray fluorescence spectrometry and scanning electron microscopy (SEM) with energy dispersive spectrometry (EDS) analysis methods for Sn and Pb amounts in solder and coatings. Test methods are needed by laboratories that perform destructive physical analysis of high‐reliability electronics for MIL‐STD‐1580B. Calibrants are prepared by evaporative deposition of multiple, alternating quantities of pure Sn and pure Pb having mass per unit area proportional to mass fractions of Sn and Pb in a solder being mimicked. Validation reference materials are prepared by evaporative deposition of thin films of SRM 1729 Tin Alloy (97Sn–3Pb). Films are created on high‐purity Ni foil to mimic some actual electronics structures and prevent charging during SEM‐EDS measurements. Maximum thickness of films prepared this way must be kept below approximately 1 µm to ensure that the entire thickness is probed by the primary X‐ray or electron beam and that measured X‐rays come from the entire thickness of all films. Detailed procedures are presented, and method performance was characterized. The primary purpose is to create calibrations for Sn and Pb that are simple to implement and establish traceability to the international system of units. The secondary purpose is to validate calibrations using a certified reference material to prove that, for simpler structures of thin solder coatings on metal, both X‐ray fluorescence and SEM‐EDS provide accurate results. Keeping films thin may be unrealistic in comparison with some, if not many, electronic structures, but this approach enables a laboratory to demonstrate competence in a controlled manner. Copyright © 2014 John Wiley & Sons, Ltd.