Simultaneous Determination of Coating Thickness and Impurity Elements in Spherical Nb-coated Zirconia Particles by Cryogenic LA-ICP-MS

Coating thickness and impurity elements content can critically affect the performance of coated materials.In this work, a novel method based on cryogenic laser ablation inductively couple plasma mass spectrometry (Cryogenic LA-ICP-MS) for simultaneous determination of niobium (Nb) coating thickness and impurity element content in zirconia particles was developed.Cryogenic ablation cell (-25 ) was employed to minimize the impact of thermal effects during the laser drilling through coating interface.Correlating SEM-measured thicknesses of hemispherical standards with their LA-ICP-MS-derived ablation times yielded an average ablation rate (AAR) of 0.3714 m/s (or 0.0743 m/pulse) under the optimized conditions (laser energy density: 6 J/cm, laser spot size: 44 m).Coating thickness was accurately measured with the relative errors < 5.52% (vs the reference values).Result of coating thicknesses for sixty particles ranged from 5.96 to 40.64 m (avg.16.66 m).Quantitative analysis of impurities in both the Nb coating and ZrO core was achieved using NIST 610 as external calibration standard with Nb/Zr internal standardization, providing detection limits from 0.003 g/g (Ta) to 389 g/g (Si).